4'-Hydroxyacetophenone 99-93-4

Details:

Product introduction:

Density	1.109
Melting Point	132-135°C(lit.)
Boling Point	147-148°C3mm Hg(lit.)
Flash Point	166 °C
JECFA Number	2040
Water Solubility	10 g/L (22 ºC)
Solubility	Soluble in ethanol and ether, slightly soluble in water
Vapor Presure	0.002Pa at 20℃
Appearance	White to off-white (Solid)
Specific Gravity	1.109
Color	Almost white to beige
BRN	774355
pKa	8.05(at 25℃)
Storage Condition	Store below +30°C.
Sensitive	Easily absorbing moisture
Refractive Index	1.5577 (estimate)
MDL	MFCD00002359
Physical and Chemical Properties	White crystals soluble in hot water, methanol, ether, acetone, insoluble in petroleum ether
Use	Raw materials for the manufacture of choleretic drugs and other organic synthesis

Overview	p-hydroxyacetophenone, because its molecule contains hydroxyl and ketone groups on the benzene ring, therefore, it is often used as an intermediate in organic synthesis to react with other compounds to synthesize many important substances. Generally used for the synthesis of pharmaceutical intermediates (α-bromo-p-hydroxyacetophenone, choleretic drugs, antipyretic analgesics and other drugs), Other (spices, feed, etc.; Pesticides, dyes, liquid crystal materials, etc.).
Application	p-hydroxyacetophenone is white needle-like crystal at room temperature, naturally occurring in the stems and leaves of Artemisia scoparia, in the roots of plants such as ginseng baby Vine. It can be used in the manufacture of choleretic drugs and other raw materials for organic synthesis.
preparation	a synthesis method of p-hydroxyacetophenone is carried out according to the following steps:(1) esterification reaction: In a 500ml reaction flask, 60g(0.63mol) of phenol and 70.0g(0.68mol) of acetic anhydride are added, stirred, cooled to 10 ℃, and the first drop of concentrated sulfuric acid is added dropwise, after the reaction is reduced to normal temperature, the second drop of concentrated sulfuric acid is added dropwise. The amount of concentrated sulfuric acid added twice is 0.5g, after cooling to 60~70 ℃, the acetic acid was distilled off under reduced pressure, the reaction solution was poured into 3 times the amount of water, adjusted to pH 8~9 with 5% sodium hydroxide, and extracted with ethyl acetate for 3 times, the extracts were combined, dried with anhydrous magnesium sulfate, filtered and concentrated to obtain 84.3g of phenyl acetate liquid, with a yield of 94.6%; Divided into three parts for standby use;(2)Fries rearrangement: take step (1) 27.2g(0.2mol) of the obtained phenyl acetate was placed in a 40.0 mL reaction flask, 30ml of O-dichlorobenzene was added under stirring, and 0.3g (mol) of aluminum trichloride was slowly added below 10 °c, temperature increased to 8 Reaction was carried out at 0 ℃ for 3.5 hours, and the reaction was completed by HPLC; Then it was reduced to 50~60 ℃, and water was slowly added for steam distillation; The distillate was separated into layers to obtain an O-dichlorobenzene layer containing O-hydroxyacetophenone, drying, filtration, for subsequent feeding; Residual liquid and activated carbon while hot filtration, cooling crystallization, filtration, P-hydroxyacetophenone white solid 11.8g, purity 99.3%, yield 43.3%;(3) the first cycle: take 27.2g(0.2mol) of phenyl acetate obtained in step (1), and add the O-dichlorobenzene dry liquid containing O-hydroxyacetophenone obtained in step (2) under stirring, under the condition of lower than 10 ℃, 40.0g(0.3mol) of aluminum trichloride is slowly added, and the mixture is heated to 80 ℃ and reacted for 3.5 hours, and the reaction of all raw materials is finished by HPLC detection; then it is reduced to 50~60 ℃, water is slowly added for steam distillation; The distillate is stratified to obtain an O-dichlorobenzene layer containing O-hydroxyacetophenone, dried and filtered for subsequent feeding; The residual liquid is filtered while hot with activated carbon, concentration, cooling crystallization, filtration, P-hydroxyacetophenone white solid 14.1g, purity 99.6%, yield 51.9%;(4) the second Secondary cycle: the process is the same as that of the first cycle. Take 27.2g (0.2mol) of phenyl acetate obtained in step (1) and add the layered dry liquid of O-dichlorobenzene layer containing O-hydroxyacetophenone after the first cycle to react, P-hydroxyacetophenone white solid 14.8g, purity 99.7%, yield 54.3%;(5) step (2)~(4) three times the white solid reaction is combined, that is, the final product, that is, 40.7g of p-hydroxyacetophenone;(6) step (4) the O-dichlorobenzene layer containing O-hydroxyacetophenone after being separated by steam distillation is extracted twice with 5% sodium hydroxide solution, and then the layers are separated, the aqueous layers were combined and adjusted to pH 3-4 with 10% hydrochloric acid; The aqueous layers were extracted twice with ethyl acetate, combined and dried, filtered and concentrated, and then purified to obtain 14.7g of O-hydroxyacetophenone.
purpose	raw materials for the manufacture of cholagogue and other organic synthesis This product is an intermediate of organic synthesis, for the production of spices. P-hydroxyacetophenone is also a choleretic. raw materials of medicine, perfume and organic synthesis as intermediates of organic synthesis, they can be used in the production of perfume. The synthesis of a-bromo-p-hydroxyacetophenone, which is mainly used, is an important intermediate for the synthesis of a selective B l receptor blocker-Atenolol (#1).
production method	is derived from the acylation and translocation of phenol. Phenol and acetyl chloride were mixed and heated slowly until the evolution of hydrogen chloride ceased to yield crude phenyl acetate. Nitrobenzene was added thereto, and aluminum trichloride was added under cooling, followed by stirring at room temperature for 2-3 hours. It was then poured into cold water and 1:3 hydrochloric acid was added until clear. Extraction with diethyl ether, recovery of diethyl ether from the extract, followed by steam distillation, nitrobenzene and O-hydroxyacetophenone by-product are distilled off at any time with steam, and p-hydroxyacetophenone remains in the residue. The residue is extracted with diethyl ether, the ether is recovered, and the crude product is obtained by cooling and crystallizing, and the product is recrystallized with water. In the above acylation operation, acetic anhydride can be used instead of acetyl chloride, and phenol and acetic anhydride are heated to reflux for 3H to form phenyl acetate in a yield of about 83%. No solvent may be used for the translocation under the action of anhydrous aluminum trichloride. In addition, P-hydroxyacetophenone can also be obtained by diazotization and hydrolysis of p-aminoacetophenone with sodium nitrite.

 

Our company specializes in processing and selling chemical raw materials, chemical products, pharmaceutical intermediates, veterinary medicine intermediates, dye intermediates, pigments, cosmetics raw materials and chemical reagents,  

Our company has a number of sales team, service and information feedback vertical integration of a sound marketing network, products are sold throughout the country and exported to South Asia, Europe, America, Africa and other more than 20 countries and regions.  

Companies adhering to the "pursuit of quality, innovation and development" business philosophy, to serve as a foundation, for the survival by the quality, seek development by science and technology, adhere to quilty comes first,fair price,good sense of customer service and responsibility. in the future hebei Nengqian import and export trade Co.,Ltd will always hold "integrity, innovation" business philosophy, to achieve honesty management, on the way of specialization, internationalization,  Keep moving!  

 

 

 

 

 

Our advantages: 

1, High quality with competitive price:

1) Standard:BP/USP/EP/Enterprise standard

2) All Purity≥99%

3) We are manufacturer and can provide high quality products with factory price.

 2, Fast and safe delivery

1) Parcel can be sent out in 24 hours after payment.Tracking number available

2) Secure and discreet shipment.Various transportation methods for your choice.

3) Customs pass rate ≥99%

4) We have our own agent/remailer/distributor who can help us ship our products very fast and safe,

and we have stock in there for transferring.

Product Packaging：

1) 1kg/bag (1kg net weight, 1.1kg gross weight, packed in an aluminum foil bag)

2) 25kg/drum (25kg net weight, 28kg gross weight; Packed in a cardboard-drum with two plastic-bags inside; Drum Size: 510mm high, 360mm diameter)

 Storage：

Stored in a cool and dry well-closed container. Keep away from moisture and strong light/heat.

Delivery：

Usually within3-5 working days after full payment.

transport：

EMS,DHL, TNT, UPS ,FEDEX, BY AIR, BY SEA

DHL Express, FedEx and EMS for quantity less than 50KG, usually called as DDU service; 

Sea shipping for quantity over 500KG; And air shipping is available for 50KG above;

For high value products, please select air shipping and DHL express for safe;

Our Service:
1. Fast Delivery: We can delivery within 24 hours upon receipt of your payment.
2. Quality can be promised. Hot sell to Worldwide.
3. Payment Terms: T/T,, t/t
4. Free Sample available at any time.
5. Tracking your order at any time. Inform your order's further new situation at any time.
6. Package: Professional packing with professional materials.

FAQ: 
1.Are you a trade company or factory   
We are a  factory with our own trading company.  

2.How do you control the quality   
Our factory is equipped with professional technicians to control quality, out inspectors take sample for testing every 2 hours to ensure the quality of our production. We also accept BV, SGS or any other Third-party inspection.   

3.How long is lead time   
We deliver goods within 3 days for small order, 7-10 days for bulk order.   

4. Where is your factory located  How can I visit the factory   
 Our factory located in HEBEI, China.

5.Can i get some samples  
  Yes, we can supply free sample, but the shipping cost be paid by our customers. 

6.How to start orders or make payments  
  Proforma invoice will be sent first after confirmation of order, enclosed our bank information.Payment by T/T,  

7. How to confirm the Product Quality before placing orders  
  You can get free samples for some products,you only need to pay the shipping cost or arrange a courier to us and take the samples. 
8. How long is lead time

We deliver goods within 3 days for small order, 7-10 days for bulk order.

 

9. How do you treat quality complaint

  First of all, our quality control will reduce the quality problem to near zero. If there is a realquality problem caused by us, we will send you free goods for replacement or refund your loss.