反应详情

To a solution of 1.36 g of 4-diethoxyphosphinylmethylbenzoic acid and 0.56 g of triethylamine in 15 ml of dry THF was slowly added a solution of 0.60 g of ethyl chlorocarbonate in 2 ml of dry THF under ice-cooling with stirring. After stirring for 30 minutes under ice-cooling, ammonia gas was slowly bubbled into the mixture for 15 minutes, stirred for 2 hours at room temperature. After adding 30 ml of water, the reaction mixture was extracted with chloroform. The extract was dried over anhydrous sodium sulfate and the solvent was evaporated. The residue was subjected to silica gel column chromatography (eluent; chloroform:methanol=10:1) to give 4-diethoxyphosphinylmethylbenzamide. it was recrystallized from chloroform-benzene mixture to give 0.80 g of colorless plate crystals. mp: 177.0°-177.5° C.

1. temperaturecooling
2. stirringAfter stirring for 30 minutes under ice-
3. temperaturecooling
4. customammonia gas was slowly bubbled into the mixture for 15 minutes
5. stirringstirred for 2 hours at room temperature
6. additionAfter adding 30 ml of water
7. extractionthe reaction mixture was extracted with chloroform
8. dry with materialThe extract was dried over anhydrous sodium sulfate
9. customthe solvent was evaporated