反应详情

Dissolved in 100 ml of 1N sodium hydroxide were 6.65 g of L-thioproline, and 50 ml of water were further added to the solution. A solution of 9.10 g of 4-phenylbutanoyl chloride in 50 ml of benzene was added dropwise to the solution under stirring. Thereafter, 50 ml of 1N sodium hydroxide were further added, and the mixture was stirred for 24 hours. A benzene layer was removed, and a water layer was washed twice with 70 ml of ether. After 7% hydrochloric acid was further added to the water layer to acidify it, the water layer was extracted three times with 70 ml of ethyl acetate. The resulting extract was dried over anhydrous sodium sulfate. Ethyl acetate was distilled off, and the resultant oily residue was subjected to column chromatography on silica gel, thereby obtaining 11.4 g of N-(4-phenylbutanoyl)-L-thioproline as colorless crystals from a chloroform-methanol fraction.

1. additionwere further added to the solution
2. stirringthe mixture was stirred for 24 hours
3. customA benzene layer was removed
4. washa water layer was washed twice with 70 ml of ether
5. additionAfter 7% hydrochloric acid was further added to the water layer
6. extractionthe water layer was extracted three times with 70 ml of ethyl acetate
7. extractionThe resulting extract
8. dry with materialwas dried over anhydrous sodium sulfate
9. distillationEthyl acetate was distilled off