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inquiryhigh quality Appearance:White or off-white Solid Storage:Sealed, dry, microtherm , avoid light and smell. Package:According to the demand of customer Application:Organic synthesis Transportation:by air or by sea Port:shanghai
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inquiryAs a leading manufacturer and supplier of chemicals in China, DayangChem not only supply popular chemicals, but also DayangChem’s R&D center offer custom synthesis services. DayangChem can provide different quantities of custom synthesis
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inquiryOur main production base is located in Xuzhou industry park. We are certified both to the ISO 9001 and ISO 14001 Standards, have a safety management system in place.Our R&D team masters core technology for process-design of target building block
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inquiryOur advantages: 1. All inquiries will be replied within 12 hours. 2. Dedication to quality, supply & service. 3. Strictly on selecting raw materials. 4. Reasonable & competitive price, fast lead time. 5. Sample is available for your eva
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inquiryWITH US,YOUR MONEY IN SAFE,YOUR BUSINESS IN SAFE 1)Quick Response Within 12 hours; 2)Quality Guarantee: All products are strictly tested by our QC, confirmed by QA and approved by third party lab in China, USA, Canada, Germany, UK, Italy, France et
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inquiryAppearance:white to light yellow-beige powder Storage:Room temperature Package:25kg/Barrel Application:pharmaceutical intermediates Transportation:Express/Sea/Air Port:Any port in China
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inquiry1.No Less 8 years exporting experience. Clients can 100% received goods 2.Lower Price with higher quality 3,Free sample 4,We are sincerely responsible for the "product quality" and "After Service" Upbio is Specialized
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inquiryOur company has been in existence for 10 years since its establishment. We have our own unique team. The company integrates independent research and development, production and sales. We have established famous brands at home and abroad. At prese
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inquiry3-Hydroxy-2,4,5-trifluorobenzoic acid CAS:116751-24-7 Qingdao Belugas Import and Export Co., Ltd. is a scientific and technological company integrating research and development, production and trade of chemical intermediates, specializing in high q
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inquiryHello, dear friend! I'm Hansen and Allen from China. Welcome to my lookchem mall! The following is a brief introduction of our company's products and services. If you are interested in our products, please contact us by emai
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inquiryOur Advantage: high quality with competitive price High quality standard: BP/USP/EP Enterprise standard All purity customized Fast and safe delivery We have reliable forwarder who can help us deliver our goods more fast and safe. We
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inquiryBest quality & Attractive price & Professional service; Trial & Pilot & Commercial Hisunny Chemical is a leading manufacturer and supplier of chemicals in China. We develop produce and distribute high quality intermediates, specia
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inquiryHangzhou KeyingChem Co., Ltd. exported this product to many countries and regions at best price. If you are looking for the material’s manufacturer or supplier in China, KeyingChem is your best choice. Pls contact with us freely for getting det
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inquiryJ&H CHEM R&D center can offer custom synthesis according to the contract research and development services for the fine chemicals, pharmaceutical, biotechnique and some of the other chemicals. J&H CHEM has some Manufacturing base in Jia
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inquiryOur Services 1. New Molecules R&D 2. Own test center HPLC NMR GC LC-MS 3. API and Intermediates from China reputed manufacturers 4. Documents support COA MOA MSDS DMF open part Our advantages 1. Government awarded company. Top 100 enter
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inquiryA substitute for perfluorooctanoic acid, mainly used as a surfactant, dispersant, additive, etc Appearance:White solid or Colorless liquid Purity:99.3 % We will ship the goods in a timely manner as required We can provide relevant documents acc
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inquiryZibo Hangyu Biotechnology Development Co., Ltd is a leading manufacturer and supplier of chemicals in China. We develop produce and distribute high quality pharmaceuticals, intermediates, special chemicals and OLED intermediates and other fine chemi
Cas:116751-24-7
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inquiryThe above product is Ality Chemical's strong item with best price, good quality and fast supply. Ality Chemical has been focusing on the research and production of this field for over 14 years. At the same time, we are always committed to providing h
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inquiryWe are one of a few suppliers that can offer custom synthesis service of this product We are specialized in custom synthesis, chemical/pharmaceutical/ pesticides outsourcing and contract research. We are committed to prov
Cas:116751-24-7
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inquirySuperior quality, moderate price & quick delivery. Appearance:white powder Storage:Stored in cool, dry and ventilation place; Away from fire and heat Package:10g/bag,or as your request Application:Used as Pharmaceutical Intermediates Transp
Cas:116751-24-7
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inquiryProduct name: 3-Hydroxyl-2,4,5-Trifluobenzyl Acid CAS No.:116751-24-7 Molecule Formula:C7H3F3O3 Molecule Weight:192.09 Purity: 99% Package: 25kg/drum Description:White crystalline powder Manufacture Standards:Enterprise Standard
Cas:116751-24-7
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inquiryOur company was built in 2009 with an ISO certificate.In the past 6 years, we have grown up as a famous fine chemicals supplier in China and we had established stable business relationships with Samsung,LG,Merck,Thermo Fisher Scientific and so
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inquiryfactory?direct?saleAppearance:White Powder Storage:Store In Dry, Cool And Ventilated Place Package:25kg/drum, also according to the clients requirement Application:It is widely used as a thickener, emulsifier and stabilizer Transportation:By Sea Or B
Cas:116751-24-7
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inquiryShandong Mopai Biotechnology Co., LTD is a leading manufacturer and supplier of chemicals in China. We develop produce and distribute high quality pharmaceuticals, intermediates, special chemicals and OLED intermediates and other fine chemicals. W
Cas:116751-24-7
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inquiry1.Applied in food field.it can improve the immune system and prolong life. 2.Appliedin cosmetic field.it can improve the skin care. 3.Applied in pharmaceutical field.it can treat various dieases. 4.Our product quality assurance will make our customer
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inquiryAppearance:95%+ Package:R&D,Pilot run Transportation:per client require Port:Express ,Air, Sea
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inquiryWe are a Union of chemistry in China, consists of chemists,engineers, laboratories,factories in China. We organize surplus capacity of R&D and production as well as custom synthesis for chemical products and chemical business project. We are supp
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inquiryStock products, own laboratory Package:Grams, Kilograms Application:For R&D Transportation:According to customer request Port:Shanghai
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inquiry3,4,5,6-tetrafluorophthalic acid
2,4,5-trifluoro-3-hydroxybenzoic acid
Conditions | Yield |
---|---|
Stage #1: 3,4,5,6-tetrafluorophthalic acid With sodium hydroxide In water at 90℃; for 9h; Stage #2: With hydrogenchloride; tri-n-propylamine In water at 140℃; under 7500.75 Torr; for 7h; pH=1; Temperature; | 90.35% |
3,4,6-trifluoro-5-hydroxyphthalic acid
2,4,5-trifluoro-3-hydroxybenzoic acid
Conditions | Yield |
---|---|
In water | 90% |
In water | 90% |
4-methoxy-3,5,6-trifluorophthalic acid
2,4,5-trifluoro-3-hydroxybenzoic acid
Conditions | Yield |
---|---|
In water | 74% |
In water | 74% |
2,4,5-trifluoro-3-hydroxybenzoic acid
Conditions | Yield |
---|---|
With sodium hydroxide; zinc In water at 25℃; for 2h; | 1.92 g |
carbon dioxide
A
2,4,5-trifluoro-3-hydroxybenzoic acid
B
2,3,5-trifluoro-4-hydroxybenzoic acid
Conditions | Yield |
---|---|
Stage #1: triisopropyl(2,3,6-trifluorophenoxy)silane With 2,2,6,6-tetramethylpiperidinyl-lithium In diethyl ether Stage #2: carbon dioxide In diethyl ether Stage #3: With hydrogenchloride Title compound not separated from byproducts; |
carbon dioxide
A
2,4,5-trifluoro-3-hydroxybenzoic acid
B
2,3,5-trifluoro-4-hydroxybenzoic acid
Conditions | Yield |
---|---|
Stage #1: 1,2,4-trifluoro-3-(methoxymethoxy)benzene With n-butyllithium In tetrahydrofuran Stage #2: carbon dioxide In tetrahydrofuran; hexane Stage #3: With hydrogenchloride In water Title compound not separated from byproducts; | |
Stage #1: 1,2,4-trifluoro-3-(methoxymethoxy)benzene With lithium diisopropyl amide In tetrahydrofuran Stage #2: carbon dioxide In tetrahydrofuran Stage #3: With hydrogenchloride In water Title compound not separated from byproducts; |
1-bromo-2,3,5-trifluoro-4-(methoxymethoxy)benzene
2,4,5-trifluoro-3-hydroxybenzoic acid
Conditions | Yield |
---|---|
Multi-step reaction with 3 steps 1.1: 2,2,6,6-tetramethylpiperidine; potassium tert-butoxide; N,N,N',N'',N''-pentamethylenediamine / butyllithium / tetrahydrofuran; hexane / 0.75 h / -125 °C 1.2: tetrahydrofuran; hexane 2.1: HCl / H2O 3.1: 1.92 g / NaOH; zinc powder / H2O / 2 h / 25 °C View Scheme |
2,4,5-trifluoro-3-hydroxybenzoic acid
Conditions | Yield |
---|---|
Multi-step reaction with 2 steps 1: HCl / H2O 2: 1.92 g / NaOH; zinc powder / H2O / 2 h / 25 °C View Scheme |
2,3,6-trifluorophenol
2,4,5-trifluoro-3-hydroxybenzoic acid
Conditions | Yield |
---|---|
Multi-step reaction with 2 steps 1.1: 82 percent / imidazole / dimethylformamide / 20 h / 25 °C 2.1: lithium 2,2,6,6-tetramethylpiperidide / diethyl ether 2.2: diethyl ether 2.3: hydrochloric acid View Scheme | |
Multi-step reaction with 5 steps 1.1: 87 percent / N-bromosuccinimide / CHCl3 / 2 h / 0 °C 2.1: 88 percent / N-ethyldiisopropylamine / CH2Cl2 / 2 h / 25 °C 3.1: 2,2,6,6-tetramethylpiperidine; potassium tert-butoxide; N,N,N',N'',N''-pentamethylenediamine / butyllithium / tetrahydrofuran; hexane / 0.75 h / -125 °C 3.2: tetrahydrofuran; hexane 4.1: HCl / H2O 5.1: 1.92 g / NaOH; zinc powder / H2O / 2 h / 25 °C View Scheme | |
Multi-step reaction with 2 steps 1.1: 87 percent / N-ethyldiisopropylamine / CH2Cl2 / 25 °C 2.1: lithium diisopropylamide / tetrahydrofuran 2.2: tetrahydrofuran 2.3: HCl / H2O View Scheme |
4-bromo-2,3,6-trifluorophenol
2,4,5-trifluoro-3-hydroxybenzoic acid
Conditions | Yield |
---|---|
Multi-step reaction with 4 steps 1.1: 88 percent / N-ethyldiisopropylamine / CH2Cl2 / 2 h / 25 °C 2.1: 2,2,6,6-tetramethylpiperidine; potassium tert-butoxide; N,N,N',N'',N''-pentamethylenediamine / butyllithium / tetrahydrofuran; hexane / 0.75 h / -125 °C 2.2: tetrahydrofuran; hexane 3.1: HCl / H2O 4.1: 1.92 g / NaOH; zinc powder / H2O / 2 h / 25 °C View Scheme |
N-methyl-tetrafluorophthalimide
2,4,5-trifluoro-3-hydroxybenzoic acid
Conditions | Yield |
---|---|
Stage #1: N-methyl-tetrafluorophthalimide With sodium hydroxide for 10h; Reflux; Stage #2: With sulfuric acid at 70 - 105℃; for 8h; Temperature; Reagent/catalyst; | |
Multi-step reaction with 2 steps 1: sodium hydroxide; zinc(II) chloride / water / 8 h / 100 °C / Large scale 2: hydrogenchloride / Reflux View Scheme | |
Multi-step reaction with 2 steps 1: water; zinc(II) chloride; sodium hydroxide / 8 h / 100 °C / Large scale 2: hydrogenchloride / water / Reflux View Scheme |
2,4,5-trifluoro-3-hydroxybenzoic acid
Conditions | Yield |
---|---|
With hydrogenchloride Reflux; | |
With hydrogenchloride In water Reflux; |
ethyl iodide
2,4,5-trifluoro-3-hydroxybenzoic acid
ethyl 3-ethoxy-2,4,5-trifluorobenzoate
Conditions | Yield |
---|---|
With sodium hydride In N,N-dimethyl-formamide for 18h; | 92% |
2,4,5-trifluoro-3-hydroxybenzoic acid
methyl iodide
methyl 3-methoxy-2,4,5-trifluorobenzoate
Conditions | Yield |
---|---|
With sodium hydride In N,N-dimethyl-formamide for 18h; | 91% |
With sodium hydride In N,N-dimethyl-formamide |
2,4,5-trifluoro-3-hydroxybenzoic acid
carbonic acid dimethyl ester
methyl 3-methoxy-2,4,5-trifluorobenzoate
2,4,5-trifluoro-3-hydroxybenzoic acid methyl ester
Conditions | Yield |
---|---|
With potassium iodide In N,N-dimethyl acetamide; water | 91% |
2,4,5-trifluoro-3-hydroxybenzoic acid
carbonic acid dimethyl ester
3-methoxy-2,4,5-trifluorobenzoic acid
Conditions | Yield |
---|---|
With potassium dihydrogenphosphate; N-ethyl-N,N-diisopropylamine In water at 170℃; for 8h; Reagent/catalyst; Solvent; Temperature; Autoclave; | 85.2% |
Stage #1: 2,4,5-trifluoro-3-hydroxybenzoic acid; carbonic acid dimethyl ester With sodium hydroxide at 55 - 60℃; for 2h; pH=8 - 10; Large scale; Stage #2: With hydrogenchloride In water at 35℃; Large scale; | 85% |
methanol
2,4,5-trifluoro-3-hydroxybenzoic acid
2,4,5-trifluoro-3-hydroxybenzoic acid methyl ester
Conditions | Yield |
---|---|
sulfuric acid at 70℃; for 18h; Sealed tube; Heating / reflux; | 79% |
2,4,5-trifluoro-3-hydroxybenzoic acid
methyl 3-methoxy-2,4,5-trifluorobenzoate
2,4,5-trifluoro-3-hydroxybenzoic acid methyl ester
Conditions | Yield |
---|---|
With dmap; potassium iodide In water; carbonic acid dimethyl ester | 78% |
2-(tert-butyldimethylsilyloxy)ethyl bromide
2,4,5-trifluoro-3-hydroxybenzoic acid
2-{[(1,1-dimethylethyl)(dimethyl)silyl]oxy}ethyl-3-[(2-{[(1,1-dimethylethyl)(dimethyl)siyl]oxy}ethyl)oxy]-2,4,5-trifluorobenzoate
Conditions | Yield |
---|---|
With potassium carbonate In N,N-dimethyl-formamide at 70℃; for 15h; | 23% |
2,4,5-trifluoro-3-hydroxybenzoic acid
2,4,5-Trifluoro-3-hydroxy-benzoyl chloride
Conditions | Yield |
---|---|
With oxalyl dichloride; N,N-dimethyl-formamide In dichloromethane at 0 - 20℃; |
2,4,5-trifluoro-3-hydroxybenzoic acid
3-ethoxy-2,4,5-trifluorobenzoyl chloride
Conditions | Yield |
---|---|
Multi-step reaction with 3 steps 1: 92 percent / NaH / dimethylformamide / 18 h 2: 79 percent / 1.0 N aq. NaOH / methanol / 3 h / Ambient temperature 3: oxalyl chloride, DMF / CH2Cl2 / 18 h / Ambient temperature View Scheme |
2,4,5-trifluoro-3-hydroxybenzoic acid
3-ethoxy-2,4,5-trifluorobenzoic acid
Conditions | Yield |
---|---|
Multi-step reaction with 2 steps 1: 92 percent / NaH / dimethylformamide / 18 h 2: 79 percent / 1.0 N aq. NaOH / methanol / 3 h / Ambient temperature View Scheme |
2,4,5-trifluoro-3-hydroxybenzoic acid
ethyl (3-ethoxy-2,4,5-trifluorobenzoyl)acetate
Conditions | Yield |
---|---|
Multi-step reaction with 4 steps 1: 92 percent / NaH / dimethylformamide / 18 h 2: 79 percent / 1.0 N aq. NaOH / methanol / 3 h / Ambient temperature 3: oxalyl chloride, DMF / CH2Cl2 / 18 h / Ambient temperature 4: 1.) n-BuLi, 2,2'-bipyridyl / 1.) THF, hexane, from -20 deg C to -5 deg C, 2.) THF, hexane, -30 deg C, 2 h View Scheme |
2,4,5-trifluoro-3-hydroxybenzoic acid
Conditions | Yield |
---|---|
Multi-step reaction with 5 steps 1: 92 percent / NaH / dimethylformamide / 18 h 2: 79 percent / 1.0 N aq. NaOH / methanol / 3 h / Ambient temperature 3: oxalyl chloride, DMF / CH2Cl2 / 18 h / Ambient temperature 4: 1.) n-BuLi, 2,2'-bipyridyl / 1.) THF, hexane, from -20 deg C to -5 deg C, 2.) THF, hexane, -30 deg C, 2 h 5: acetic anhydride / 18 h / Heating View Scheme |
2,4,5-trifluoro-3-hydroxybenzoic acid
(Z)-3-Cyclopropylamino-2-(3-ethoxy-2,4,5-trifluoro-benzoyl)-acrylic acid ethyl ester
Conditions | Yield |
---|---|
Multi-step reaction with 6 steps 1: 92 percent / NaH / dimethylformamide / 18 h 2: 79 percent / 1.0 N aq. NaOH / methanol / 3 h / Ambient temperature 3: oxalyl chloride, DMF / CH2Cl2 / 18 h / Ambient temperature 4: 1.) n-BuLi, 2,2'-bipyridyl / 1.) THF, hexane, from -20 deg C to -5 deg C, 2.) THF, hexane, -30 deg C, 2 h 5: acetic anhydride / 18 h / Heating 6: ethanol / 18 h View Scheme |
2,4,5-trifluoro-3-hydroxybenzoic acid
5-amino-1-cyclopropyl-6,7-difluoro-1,4-dihydro-8-ethoxy-4-oxo-3-quinolinecarboxylic acid
Conditions | Yield |
---|---|
Multi-step reaction with 10 steps 1: 92 percent / NaH / dimethylformamide / 18 h 2: 79 percent / 1.0 N aq. NaOH / methanol / 3 h / Ambient temperature 3: oxalyl chloride, DMF / CH2Cl2 / 18 h / Ambient temperature 4: 1.) n-BuLi, 2,2'-bipyridyl / 1.) THF, hexane, from -20 deg C to -5 deg C, 2.) THF, hexane, -30 deg C, 2 h 5: acetic anhydride / 18 h / Heating 6: ethanol / 18 h 7: NaH / tetrahydrofuran / 5 h / Ambient temperature 8: 61 percent / KNO3, conc. H2SO4 / 18 h / Ambient temperature 9: 89 percent / H2 / Raney nickel / tetrahydrofuran / 4 h / 24 - 30 °C / 1241.2 - 1551.4 Torr 10: 90 percent / 1.0 N aq. NaOH / ethanol / 18 h / Ambient temperature View Scheme |
2,4,5-trifluoro-3-hydroxybenzoic acid
ethyl 1-cyclopropyl-6,7-difluoro-1,4-dihydro-8-ethoxy-4-oxo-3-quinolinecarboxylate
Conditions | Yield |
---|---|
Multi-step reaction with 7 steps 1: 92 percent / NaH / dimethylformamide / 18 h 2: 79 percent / 1.0 N aq. NaOH / methanol / 3 h / Ambient temperature 3: oxalyl chloride, DMF / CH2Cl2 / 18 h / Ambient temperature 4: 1.) n-BuLi, 2,2'-bipyridyl / 1.) THF, hexane, from -20 deg C to -5 deg C, 2.) THF, hexane, -30 deg C, 2 h 5: acetic anhydride / 18 h / Heating 6: ethanol / 18 h 7: NaH / tetrahydrofuran / 5 h / Ambient temperature View Scheme |
2,4,5-trifluoro-3-hydroxybenzoic acid
ethyl 5-amino-1-cyclopropyl-6,7-difluoro-1,4-dihydro-8-ethoxy-4-oxo-3-quinolinecarboxylate
Conditions | Yield |
---|---|
Multi-step reaction with 9 steps 1: 92 percent / NaH / dimethylformamide / 18 h 2: 79 percent / 1.0 N aq. NaOH / methanol / 3 h / Ambient temperature 3: oxalyl chloride, DMF / CH2Cl2 / 18 h / Ambient temperature 4: 1.) n-BuLi, 2,2'-bipyridyl / 1.) THF, hexane, from -20 deg C to -5 deg C, 2.) THF, hexane, -30 deg C, 2 h 5: acetic anhydride / 18 h / Heating 6: ethanol / 18 h 7: NaH / tetrahydrofuran / 5 h / Ambient temperature 8: 61 percent / KNO3, conc. H2SO4 / 18 h / Ambient temperature 9: 89 percent / H2 / Raney nickel / tetrahydrofuran / 4 h / 24 - 30 °C / 1241.2 - 1551.4 Torr View Scheme |
2,4,5-trifluoro-3-hydroxybenzoic acid
ethyl 1-cyclopropyl-6,7-difluoro-1,4-dihydro-8-ethoxy-5-nitro-4-oxo-3-quinolinecarboxylate
Conditions | Yield |
---|---|
Multi-step reaction with 8 steps 1: 92 percent / NaH / dimethylformamide / 18 h 2: 79 percent / 1.0 N aq. NaOH / methanol / 3 h / Ambient temperature 3: oxalyl chloride, DMF / CH2Cl2 / 18 h / Ambient temperature 4: 1.) n-BuLi, 2,2'-bipyridyl / 1.) THF, hexane, from -20 deg C to -5 deg C, 2.) THF, hexane, -30 deg C, 2 h 5: acetic anhydride / 18 h / Heating 6: ethanol / 18 h 7: NaH / tetrahydrofuran / 5 h / Ambient temperature 8: 61 percent / KNO3, conc. H2SO4 / 18 h / Ambient temperature View Scheme |
2,4,5-trifluoro-3-hydroxybenzoic acid
Conditions | Yield |
---|---|
Multi-step reaction with 11 steps 1: 92 percent / NaH / dimethylformamide / 18 h 2: 79 percent / 1.0 N aq. NaOH / methanol / 3 h / Ambient temperature 3: oxalyl chloride, DMF / CH2Cl2 / 18 h / Ambient temperature 4: 1.) n-BuLi, 2,2'-bipyridyl / 1.) THF, hexane, from -20 deg C to -5 deg C, 2.) THF, hexane, -30 deg C, 2 h 5: acetic anhydride / 18 h / Heating 6: ethanol / 18 h 7: NaH / tetrahydrofuran / 5 h / Ambient temperature 8: 61 percent / KNO3, conc. H2SO4 / 18 h / Ambient temperature 9: 89 percent / H2 / Raney nickel / tetrahydrofuran / 4 h / 24 - 30 °C / 1241.2 - 1551.4 Torr 10: 90 percent / 1.0 N aq. NaOH / ethanol / 18 h / Ambient temperature 11: 1.) Et3N, 2.) TFA / 1.) DMSO, CH3CN, RT, 18 h, 2.) CH2Cl2, from 0 deg C to RT, 1 h View Scheme |
2,4,5-trifluoro-3-hydroxybenzoic acid
Conditions | Yield |
---|---|
Multi-step reaction with 11 steps 1: 92 percent / NaH / dimethylformamide / 18 h 2: 79 percent / 1.0 N aq. NaOH / methanol / 3 h / Ambient temperature 3: oxalyl chloride, DMF / CH2Cl2 / 18 h / Ambient temperature 4: 1.) n-BuLi, 2,2'-bipyridyl / 1.) THF, hexane, from -20 deg C to -5 deg C, 2.) THF, hexane, -30 deg C, 2 h 5: acetic anhydride / 18 h / Heating 6: ethanol / 18 h 7: NaH / tetrahydrofuran / 5 h / Ambient temperature 8: 61 percent / KNO3, conc. H2SO4 / 18 h / Ambient temperature 9: 89 percent / H2 / Raney nickel / tetrahydrofuran / 4 h / 24 - 30 °C / 1241.2 - 1551.4 Torr 10: 90 percent / 1.0 N aq. NaOH / ethanol / 18 h / Ambient temperature 11: 1.) Et3N, 2.) TFA / 1.) DMSO, CH3CN, RT, 18 h, 2.) CH2Cl2, from 0 deg C to RT, 1 h View Scheme |
2,4,5-trifluoro-3-hydroxybenzoic acid
Conditions | Yield |
---|---|
Multi-step reaction with 11 steps 1: 92 percent / NaH / dimethylformamide / 18 h 2: 79 percent / 1.0 N aq. NaOH / methanol / 3 h / Ambient temperature 3: oxalyl chloride, DMF / CH2Cl2 / 18 h / Ambient temperature 4: 1.) n-BuLi, 2,2'-bipyridyl / 1.) THF, hexane, from -20 deg C to -5 deg C, 2.) THF, hexane, -30 deg C, 2 h 5: acetic anhydride / 18 h / Heating 6: ethanol / 18 h 7: NaH / tetrahydrofuran / 5 h / Ambient temperature 8: 61 percent / KNO3, conc. H2SO4 / 18 h / Ambient temperature 9: 89 percent / H2 / Raney nickel / tetrahydrofuran / 4 h / 24 - 30 °C / 1241.2 - 1551.4 Torr 10: 90 percent / 1.0 N aq. NaOH / ethanol / 18 h / Ambient temperature 11: 1.) Et3N, 2.) TFA / 1.) DMSO, CH3CN, RT, 18 h, 2.) CH2Cl2, from 0 deg C to RT, 1 h View Scheme |
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