反应详情

A solution of 15.2 g of ethyl 3-(p-chlorobenzoyl)-benzyl malonate in 50 ml of acetic acid was added to a solution of 50 ml of sulfuric acid and 50 ml of water and the mixture was refluxed under a nitrogen atmosphere for 20 hours and then cooled to room temperature. The mixture was poured into water and then extracted with methylene chloride. The organic phase was extracted with N sodium hydroxide and the alkaline phase was treated with activated carbon, filtered and acidified by addition at 10° C with stirring of 270 ml of N hydrochloric acid. The mixture was vacuulm filtered and the precipitate was washed with water and dried under reduced pressure to obtain 3.11 g of 3-(3'-p-chlorobenzyl-phenyl)-propionic acid which was used as is for the next step.

1. temperaturethe mixture was refluxed under a nitrogen atmosphere for 20 hours
2. extractionextracted with methylene chloride
3. extractionThe organic phase was extracted with N sodium hydroxide
4. additionthe alkaline phase was treated with activated carbon
5. filtrationfiltered
6. additionacidified by addition at 10° C
7. filtrationThe mixture was vacuulm filtered
8. washthe precipitate was washed with water
9. customdried under reduced pressure