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inquirypotassium acetylacetonate
iron(III)-acetylacetonate
Conditions | Yield |
---|---|
In ethanol at pH 5-6 by the method of Fackler, Progress in Inorganic Chemistry, 1966, 7, 403; subliming twice (t=180 °C, P=5E-2 torr); elem. anal.; | 95% |
Conditions | Yield |
---|---|
With ammonia In water anhyd. FeCl3 dissolved in water, excess ammonia soln. added slowly withstirring and mixt heated on steam-bath for 15-20 min, Fe(OH)3 filtered off, washed with water and heated with acetylacetone on steam-bath for 35 min.; mixt. cooled, crystalsdried and recrystd. from ethanol; elem. anal.; | 90% |
In water Aq. FeCl3 soln. was added to acetylacetone under stirring, mixt. was heated on a water bath, slight excess of NH4OH was added during stirring in hot conditions; crystals were filtered, washed with water, dried and recrystd. from CHCl3; | 37% |
With sodium acetate In ethanol; water to aq. soln. of FeCl3 and sodium acetate alc. soln. of acetylacetonate was added;; recrystn. (ether or alc.);; |
iron(III) chloride
sodium (Z)-4-oxopent-2-en-2-olate
iron(III)-acetylacetonate
Conditions | Yield |
---|---|
In solid byproducts: NaCl; mechanical treatment of the react. mixt. (FeCl3 (1.18 mmol) and an org.compd. (3.55 mmol)) in stainless steel reactors; the steel balls were used as an activating packing; in a dry box under N2; self-propagating synthesis; isolation by sublimation or extn.; elem. anal.; IR-spectroscopy; X-ray diffraction; | 80% |
In benzene byproducts: NaCl; a react. of FeCl3 and an org. compd. in the ratio 1:3; under N2; stirring for 2 d; elem. anal.; IR-spectroscopy; X-ray diffraction; | 60% |
Conditions | Yield |
---|---|
With tert-butylammonium hexafluorophosphate(V) In acetylacetone Electrochem. Process; tetra-n-butylammonium hexafluorophosphate added to dry acetylacetone, Feelectrode, 300 V, 10-50 mA, ca. 10 h; evapd. under vac., solid washed twice with hexane and twice with petroleum ether; | 75.7% |
Conditions | Yield |
---|---|
In ethanol; dichloromethane for 0.5h; | 73% |
Conditions | Yield |
---|---|
In toluene; Petroleum ether byproducts: 2-ethylhexanoic acid; a soln. of Fe-salt in petrol ether was added dropwise to a warm soln. (70-80°C) of dione in dry toluene under stirring, cooled; filtered, recrystd. from toluene, petrole ether or a mixt. of both solvents; | 70% |
iron(III)-acetylacetonate
Conditions | Yield |
---|---|
With sodium hydroxide; acetylacetone In water Kinetics; byproducts: {Fe(CN)6}(4-), NO, HONC(COCH3)2; addn. of NaOH to a soln. of pentane-2,4-dione and Na2{Fe(CN)5(NO)} in water, standing in the dark for 3 h (mechanism discussed); filtration of crystals; | 16% |
Conditions | Yield |
---|---|
With potassium hydroxide at 0 - 20℃; for 0.75h; Neat (no solvent); |
Conditions | Yield |
---|---|
In neat (no solvent) | |
Irradiation (UV/VIS); | |
Irradiation (UV/VIS); |
Conditions | Yield |
---|---|
In methanol iron(III)chloride hexahydrate, acetylacetone, sodium acetate trihydrate and methanol used, according to J. D. Woolines (Ed.) Metal Acetylacetonate Complexes by C. Gildewell, VCH, Weinheim. 1994, pp 116-121; | |
With CH3COONa In methanol; water soln. of acetylacetonate in methanol added to soln. of FeCl3*6H2O in water; soln. of CH3COONa added; heated at 50°C; cooled for 24 h at 4°C; filtered; washed (water); recrystd. (toluene); |
acetylacetone
iron(III)-acetylacetonate
Conditions | Yield |
---|---|
With sodium hydrogencarbonate In water Room temp.;; |
Conditions | Yield |
---|---|
In diethyl ether metathesis; waterfree FeCl3; dry ether;; | |
In diethyl ether metathesis; waterfree FeCl3; dry ether;; |
Conditions | Yield |
---|---|
With acetylacetone In ethanol Fernelius methode (according to W. C. Fernelius, Inorganic Synthesis, Vol2, McGraw-Hill Publ. Co, New York 1946 (p. 10)); pptn. from soln.; |
Conditions | Yield |
---|---|
In water small excess of acetylacetone (24 hours); pptn.;; recrystn.: twice from benzene;; | |
In water small excess of acetylacetone (24 hours); pptn.;; recrystn.: twice from benzene;; | |
In neat (no solvent) Heating; |
Conditions | Yield |
---|---|
Irradiation (UV/VIS); small amounts of Fe(II) compound;; | |
Irradiation (UV/VIS); small amounts of Fe(II) compound;; |
Conditions | Yield |
---|---|
without formation of hydrogen;; | |
without formation of hydrogen;; |
acetylacetone
iron(III)-acetylacetonate
Conditions | Yield |
---|---|
In tetrachloromethane Kinetics; 298 K; |
Conditions | Yield |
---|---|
With acetylacetone In benzene byproducts: isopropanol; anhydrous conditions; molar ratio=1:12; distn.; |
Conditions | Yield |
---|---|
In benzene-d6 for 0.166667h; Solvent; Inert atmosphere; |
Conditions | Yield |
---|---|
Stage #1: iron(III) chloride In ethanol at 110 - 130℃; for 4h; Stage #2: acetylacetone With sodium acetate for 24h; Reagent/catalyst; |
Conditions | Yield |
---|---|
Stage #1: iron(III) chloride hexahydrate With potassium hydroxide In water pH=8; Stage #2: acetylacetone In methanol; water at 70 - 75℃; for 0.333333h; |
iron(III)-acetylacetonate
Conditions | Yield |
---|---|
With alkali In water immediate pptn.;; | 100% |
With alkali In water immediate pptn.;; | 100% |
In water on boiling;; | |
In water on boiling;; |
iron(III)-acetylacetonate
tris(2-mercaptoethyl)amine
carbon monoxide
[Fe(Fe(CO)(N(CH2CH2S)3))2]
Conditions | Yield |
---|---|
In acetonitrile (N2); using Schlenk techniques; stirring of soln. of (Fe(acac)3) (2 mmol) and N(CH2CH2SH)3 (3 mmol) in MeCN under CO atmosphere for 20 min (two thirds of mol of CO per mol of Fe); | 100% |
In dimethyl sulfoxide (N2); using Schlenk techniques; stirring of soln. of (Fe(acac)3) (2 mmol) and N(CH2CH2SH)3 (3 mmol) in dmso under CO atmosphere for 20 min (two thirds of mol of CO per mol of Fe); filtration under CO; pptn.; elem. anal.; | 59% |
In dimethyl sulfoxide (N2); using Schlenk techniques; mixing of soln. of (Fe(acac)3) (0.5 mmol) in MeCN and N(CH2CH2SH)3 (0.5 mmol) in MeCN; evacuation and filling with CO atmosphere for week (two thirds of mol of CO per mol of Fe); filtration under CO; crystn., filtration, washing with ether, drying in vac.; | |
In N,N-dimethyl-formamide (N2); using Schlenk techniques; mixing of soln. of (Fe(acac)3) and N(CH2CH2SH)3 in DMF under CO atmosphere (two thirds of mol of CO per mol of Fe); |
iron(III)-acetylacetonate
diethyldithiophosphinic acid
Conditions | Yield |
---|---|
In not given stoich. mixt. in solvent (benzene, toluene, acetone, ethanol, butanol orchloroform) refluxing for 3-4 h; solid sepn. by filtration, washing several times with EtOH, drying at 105°C to const. weight; elem. anal., TG, DTG, DTA; | 99% |
In neat (no solvent) stoich. mixt. heating a little over m.p. of the acid for 3-4 h; solid sepn. by filtration, washing several times with EtOH, drying at 105°C to const. weight; elem. anal.; | 99% |
iron(III)-acetylacetonate
diphenylthiophosphinic acid
Conditions | Yield |
---|---|
In not given stoich. mixt. in solvent (benzene, toluene, acetone, ethanol, butanol orchloroform) refluxing for 3-4 h; solid sepn. by filtration, washing several times with EtOH, drying at 105°C to const. weight; elem. anal., TG, DTG, DTA; | 99% |
In neat (no solvent) stoich. mixt. heating a little over m.p. of the acid for 3-4 h; solid sepn. by filtration, washing several times with EtOH, drying at 105°C to const. weight; elem. anal.; | 99% |
Conditions | Yield |
---|---|
In not given stoich. mixt. in solvent (benzene, toluene, acetone, ethanol, butanol orchloroform) refluxing for 3-4 h; solid sepn. by filtration, washing several times with EtOH, drying at 105°C to const. weight; elem. anal., TG, DTG, DTA; | 99% |
In neat (no solvent) stoich. mixt. heating a little over m.p. of the acid for 3-4 h; solid sepn. by filtration, washing several times with EtOH, drying at 105°C to const. weight; elem. anal.; | 99% |
iron(III)-acetylacetonate
diethyl-phosphinothioic acid
Conditions | Yield |
---|---|
In not given stoich. mixt. in solvent (benzene, toluene, acetone, ethanol, butanol orchloroform) refluxing for 3-4 h; solid sepn. by filtration, washing several times with EtOH, drying at 105°C to const. weight; elem. anal., TG, DTG, DTA; | 99% |
In neat (no solvent) stoich. mixt. heating a little over m.p. of the acid for 3-4 h; solid sepn. by filtration, washing several times with EtOH, drying at 105°C to const. weight; elem. anal.; | 99% |
iron(III)-acetylacetonate
diphenylphosphinodithioic acid
Conditions | Yield |
---|---|
In neat (no solvent) stoich. mixt. heating a little over m.p. of the acid for 3-4 h; solid sepn. by filtration, washing several times with EtOH, drying at 105°C to const. weight; elem. anal.; | 99% |
In not given stoich. mixt. in solvent (benzene, toluene, acetone, ethanol, butanol orchloroform) refluxing for 3-4 h; solid sepn. by filtration, washing several times with EtOH, drying at 105°C to const. weight; elem. anal., TG, DTG, DTA; | 99% |
iron(III)-acetylacetonate
dibutylphosphinic acid
Conditions | Yield |
---|---|
In not given stoich. mixt. in solvent (benzene, toluene, acetone, ethanol, butanol orchloroform) refluxing for 3-4 h; solid sepn. by filtration, washing several times with EtOH, drying at 105°C to const. weight; elem. anal., TG, DTG, DTA; | 99% |
In neat (no solvent) stoich. mixt. heating a little over m.p. of the acid for 3-4 h; solid sepn. by filtration, washing several times with EtOH, drying at 105°C to const. weight; elem. anal.; | 99% |
iron(III)-acetylacetonate
diphenyl-phosphinic acid
Conditions | Yield |
---|---|
In not given stoich. mixt. in solvent (benzene, toluene, acetone, ethanol, butanol orchloroform) refluxing for 3-4 h; solid sepn. by filtration, washing several times with EtOH, drying at 105°C to const. weight; elem. anal., TG, DTG, DTA; | 99% |
In neat (no solvent) stoich. mixt. heating a little over m.p. of the acid for 3-4 h; solid sepn. by filtration, washing several times with EtOH, drying at 105°C to const. weight; elem. anal.; | 99% |
Conditions | Yield |
---|---|
In methanol at 40℃; for 2h; Inert atmosphere; | 99% |
In methanol at 40℃; for 2h; Inert atmosphere; | 99% |
iron(III)-acetylacetonate
2,9,16,23-tetra-tert-butylphthalocyanine
Conditions | Yield |
---|---|
With 1,8-diazabicyclo[5.4.0]undec-7-ene In 1,2-dichloro-benzene to a soln. of C32H14N8 in C6H4Cl2, DBU and Fe complex added; heated at 150°C for 1.5 h; pptd. by CH3OH; UV-vis and TLC control; detd. by MALDI-TOF mass-spectrometry; | 98% |
2,9,16,23-tetra-t-butyl-29H,31H-phthalocyanine
iron(III)-acetylacetonate
Conditions | Yield |
---|---|
With 1,8-diazabicyclo[5.4.0]undec-7-ene In 1,2-dichloro-benzene at 150℃; for 1.5h; | 98% |
Conditions | Yield |
---|---|
In methanol at 40℃; for 2h; | 98% |
iron(III)-acetylacetonate
Thiosalicylic acid
2-acetyl-3-hydroxybenzo[b]thiophene
Conditions | Yield |
---|---|
Stage #1: iron(III)-acetylacetonate; Thiosalicylic acid In ethylene glycol at 120℃; for 4h; Inert atmosphere; Stage #2: With hydrogenchloride In water; ethylene glycol at 20℃; Inert atmosphere; | 97% |
Stage #1: iron(III)-acetylacetonate; Thiosalicylic acid In ethylene glycol at 120℃; Inert atmosphere; Stage #2: With hydrogenchloride In water; ethylene glycol for 0.5h; |
Conditions | Yield |
---|---|
In methanol at 40℃; for 2h; Inert atmosphere; | 97% |
Conditions | Yield |
---|---|
In neat (no solvent) Fe(acac)3 and pyrazole were heated under N2 for 6 h at 180°C; mixt. was allowed to cool, washed with acetone and filtered; elem. anal.; | 96.6% |
iron(III)-acetylacetonate
(R,S)-2-(diphenylphosphinoyl)propanoic acid
Conditions | Yield |
---|---|
In tetrahydrofuran stirring (3 d); addn. of Et2O, standing (4°C, overnight), filtration, washing (Et2O), drying in air, recrystn. (toluene/CH2Cl2, 4°C, several d), filtration, washing (toluene), drying in air; elem. anal.; | 95% |
Conditions | Yield |
---|---|
In methanol at 40℃; for 2h; Inert atmosphere; | 95% |
iron(III)-acetylacetonate
Conditions | Yield |
---|---|
In dichloromethane | 95% |
iron(III)-acetylacetonate
1-Hexadecanol
A
4-hydroxy-5-methylpentan-2-one
B
hexadecyl acetate
C
16-hydroxyhexadecanoic acid
Conditions | Yield |
---|---|
at 80 - 300℃; under 760.051 Torr; for 2h; Green chemistry; | A n/a B n/a C n/a D 95% |
Conditions | Yield |
---|---|
In diethyl ether under Ar; a mixt. of Fe-contg. compd. (12.9 mmol) and a ligand (30.3 mmol) in Et2O was treated dropwise at ca. -20°C with a soln. of AlMe2(OMe); the mixt. was allowed to warm up to room temp. and stirred at this temp. for 12 h; the suspn. was dild. with Et2O and the solid was filtered off, washed with Et2O, C7H16 and dried in vac.; IR-, NMR spectra; | 93% |
iron(III)-acetylacetonate
5-chloro-2-mercapto-benzoic acid
1-(5-chloro-3-hydroxy-benzo[b]thiophen-2-yl)-ethanone
Conditions | Yield |
---|---|
Stage #1: iron(III)-acetylacetonate; 5-chloro-2-mercapto-benzoic acid In ethylene glycol at 120℃; Inert atmosphere; Stage #2: With hydrogenchloride In water; ethylene glycol at 20℃; Inert atmosphere; | 93% |
Conditions | Yield |
---|---|
In methanol at 40℃; for 2h; Inert atmosphere; | 93% |
iron(III)-acetylacetonate
N-methylacetohydroxamic acid
Conditions | Yield |
---|---|
In methanol at 20℃; for 2h; | 93% |
iron(III)-acetylacetonate
N(CH2CH2NHCOC5H2NCH3OOH)2(CH2CH2NHCOC6H2(OH)2CONHCH2CH2OCH3)*HCl
Conditions | Yield |
---|---|
In methanol under N2 atm. to soln. ligand in MeOH soln. KOH in MeOH was added, soln.Fe(acac)3 in MeOH was added and stirred for 1 h; soln. was concd. and added to ether, ppt. was centrifugated, solid was suspended in ether and filtered; elem. anal.; | 92.4% |
iron(III)-acetylacetonate
Conditions | Yield |
---|---|
In water portionwise addn. of equimolar amts. of Fe(acac)3 and 0.1 M KOH to 2 equiv. of ligand, stirring (room temp., 20 h); filtration, solvent removal, chromy. (Sephadex LH-20, MeOH), solvent removal; elem. anal.; | 92% |
Conditions | Yield |
---|---|
In neat (no solvent, solid phase) at 70℃; for 168h; Sealed tube; | 92% |
In hexane for 1h; Inert atmosphere; | 90% |
iron(III)-acetylacetonate
N(CH2CH2NHCOC6H2(OH)2CONHCH2CH2OCH3)3
Conditions | Yield |
---|---|
In methanol under N2 atm. to soln. ligand in MeOH soln. KOH in MeOH was added, soln.Fe(acac)3 in MeOH was added and stirred for 1 h; soln. was concd. and added to ether, ppt. was centrifugated, solid was suspended in ether and filtered; elem. anal.; | 91.7% |
iron(III)-acetylacetonate
water
μ-oxodi[iron(III)(3,6,13-tribromo-2,7,12,17-tetra-n-propylporphycenato)]
Conditions | Yield |
---|---|
With NaOH In dichloromethane reflux in phenol for 20 min, phenol was evapd. in vac., residue was dissolved in CH2Cl2, stirred with aq. NaOH over 1 h; soln. was washed with H2O, org. layer was dried over Na2SO4, mixt. was filtered, filtrate was concd. and dried in vac., recrysn. from CHCl3/MeOH, elem. anal.; | 91% |
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