ChemicalBook CAS DataBase List Clofibrate

Clofibrate synthesis

9synthesis methods

Product Name:Clofibrate
CAS Number:637-07-0
Molecular formula:C12H15ClO3
Molecular Weight:242.7

Clofibrate, ethyl ether 2-(4-chloropheoxy)-iso-butyric acid (20.2.2), is synthesized by esterifying 2-(4-chlorophenoxy)-iso-butyric acid (20.2.1) with ethyl alcohol. This is synthesized in a single-stage reaction from 4-chlorophenol, acetone, and chloroform in the presence of an alkali, evidently by initial formation of chlorethone-trichloro-tert-butyl alcohol, which under the reaction conditions is converted into (4-chlorophenoxy)trichlorotert- butyl ether, and further hydrolyzed to the desired acid 20.2.1, which is further esterified with ethanol in the presence of inorganic acid.

600-00-0 Synthesis

600-00-0
265 suppliers
$13.00/5g

106-48-9
478 suppliers
$10.00/5 g

637-07-0
229 suppliers
$13.00/500mg

Yield:637-07-0 96%

Reaction Conditions:

with potassium carbonate in N,N-dimethyl-formamide at 30 - 70; for 5 h;

Steps:

16
Compound III-1 (1 g, 7.779 mmol) and potassium carbonate (2.15 g, 15.56 mmol) were dissolved in N, N-dimethylformamide (10 mL).After stirring for 30 minutes at room temperature,Ethyl 2-bromo-2-methylpropanoate (3.4 mL) was added dropwise,It was then reacted at 70 ° C for 5 hours.Cool to room temperature, add water (30 mL),The aqueous phase was extracted with ethyl acetate (10 mL x 3),The organic phase was washed with saturated brine (10 mL x 3),Dry over anhydrous sodium sulfate and evaporate the solvent under reduced pressure.The residue was subjected to column chromatography (eluent: petroleum ether / ethyl acetate = 50/3),Compound III-2 was obtained (white solid, 1.8 g, yield 96%).

References:

China Pharmaceutical University;Sun Hongbin;Yan Dingfei;Feng Zhiqi;Zhang Jia;Yao Zhiying;Zhao Wenfeng;Zhang Xiangying;Sun Geng;Han Lishuai;Wu Wenzhen;Liu Shengjie;Zhao Xing;Li Minglei;Yu Shengqi;Chen Hui;Cheng Yalong;Wang Pengfei;Dai Liang;Wen Xiaoan;Liu Jun CN110372638, 2019, A Location in patent:Paragraph 0147; 0148; 0149; 0150

FullText

18672-04-3 Synthesis