반응 #64709

반응 방정식

Hydrochloric acid

N-Methylformamide

triethyl amine

2-phenoxybenzoic acid

thionyl chloride

Trichloromethylchloroformate

→

title compound

수율 61.0%

N-methyl-2-(2-phenoxyphenyl)-2-oxoacetamide

수율 61.0%

용매

acetone

Water

toluene

반응 조건

후처리

1. 1
   온도cooling
2. 2
   기타A large amount of insoluble materials were precipitated
3. 3
   workup.ADDITIONTo the mixture was added 2-phenoxybenzoyl chloride which
4. 4
   workup.STIRRINGThe resulting mixture was stirred at bath temperature of 40° to 50° C. for 26 hours
5. 5
   workup.STIRRINGthe mixture was stirred for 12 hours
6. 6
   추출was then extracted with toluene
7. 7
   기타purified by column chromatography on silica gel

실험 절차

N-Methylformamide (2.36 g, 40.0 mmol) and triethyl amine (8.08 g, 80.0 mmol) were dissolved in toluene (40 ml). Trichloromethylchloroformate (3.96 g, 20.0 mmol) was added dropwise slowly under ice-cooling while maintaining the inner temperature at 10° C. or lower. The mixture was stirred at the same temperature for 1 hour. A large amount of insoluble materials were precipitated. To the mixture was added 2-phenoxybenzoyl chloride which was prepared from 2-phenoxybenzoic acid (4.28 g, 20.0 mmol) and thionyl chloride (2.86 g, 24.0 mmol). The resulting mixture was stirred at bath temperature of 40° to 50° C. for 26 hours. 5N-Hydrochloric acid (12 ml) and acetone (20 ml) were added, and the mixture was stirred for 12 hours. Water was added to the mixture, which was then extracted with toluene and purified by column chromatography on silica gel to obtain the title compound (3.11 g, Yield: 61.0%).

출처