反应详情

To a solution of diethyl bromomalonate (10.5 g) and triethylamine (8.5 g) in methylene chloride (3.8 l), N-(2,2-dimethyl-3-mercaptopropionyl)-L-cysteine (9.5 g) dissolved in methylene chloride (0.3 l) was added dropwise under ice-salt cooling. After the addition, the reaction mixture was stirred for 30 minutes at the same temperature and for 30 minutes at room temperature. The mixture was acidified with 6N hydrochloric acid and washed with saturated sodium chloride solution. The organic layer was dried over anhydrous sodium sulfate and concentrated in vacuo. Separated crystals were collected by filtration to give 6.1 g (65%) of the titled compound.

1. additionwas added dropwise under ice-salt cooling
2. additionAfter the addition
3. washwashed with saturated sodium chloride solution
4. dry with materialThe organic layer was dried over anhydrous sodium sulfate
5. concentrationconcentrated in vacuo
6. customSeparated crystals
7. filtrationwere collected by filtration