反应详情

To a solution of 17.7 g. of 1-[3-(4-bromobenzoyl)propionyl]-L-proline (Example 36) in 150 ml. of acetic acid is added dropwise, a solution of 9.0 g. of bromine in 20 ml. of acetic acid followed by 5 drops of hydrobromic acid in acetic acid. The mixture is stirred for 18 hours, evaporated to 1/2 its volume, poured into 300 ml. of ice water and extracted with methylene chloride. The organic extract is washed twice with water, once with saturated sodium chloride solution, dried over magnesium sulfate, clarified with charcoal and evaporated to dryness in vacuo. The desired product is recovered as 20.5 g. of a white amorphous solid.

1. customevaporated to 1/2 its volume
2. additionpoured into 300 ml
3. extractionof ice water and extracted with methylene chloride
4. extractionThe organic extract
5. washis washed twice with water, once with saturated sodium chloride solution
6. dry with materialdried over magnesium sulfate
7. customevaporated to dryness in vacuo
8. customThe desired product is recovered as 20.5 g