Diclofenac Related Compound 7 synthesis

Yield: 91%

Reaction Conditions:

Stage #1:chloroacetyl chloride;aniline in benzene at 20; for 3 h;Reflux;
Stage #2:2,6-Dichlorophenol with sodium carbonate in benzene at 80; for 24 h;Temperature;

Steps:

1.1 Preparation of 2-(2,6-dichlorophenoxy)-N-phenylacetamide (Compound II)
Chloroacetyl chloride (122 g, 1.08 mol) was added dropwise to the reaction solution under stirring at 20 ° C, and the reaction was refluxed for 3 hours (10 g, 1.07 mol), benzene (626.5 g, 8.02 mol) (127 g, 1.63 mol) was added to the reaction solution, 19 g of a catalyst (PEG-400), 2,6-dichlorophenol (175 g, 1.07 mol), sodium carbonate (78 g, 0.74 mol) (Compound II: 2- (2,6-dichlorophenoxy) - (2-methyl-2- (2,6-dichlorophenoxy) - 2-methyl-2- N-phenylacetamide) in 91% yield.

References:

Jilin University;Liaoyuan Yinying Pharmaceutical Co., Ltd.;Li Guiying;Wang Zhaokun;Li Shumei;Peng Xiaojuan;Jin Xingtong CN106905178, 2017, A Location in patent:Paragraph 0021; 0037-0039