反应详情

温度

-15 °C

A solution of 15.7 g (0.0266 mole) of Boc-N-methyl-L-leucyl-L-valyl-N-methyl-L-alanyl-L-alanine benzyl ester in 125 ml of dry dichloromethane was stirred and cooled to -10° C. while 70 ml trifluoroacetic acid, previously cooled at -15° C., was added. After 2 hours, the reaction was carefully added with good stirring to a mixture of 105 g of sodium bicarbonate, ice, and 200 ml of dichloromethane. The organic layer was separated and the aqueous layer was extracted with another 50 ml of dichloromethane. The combined organic layers were washed with 3×80 ml of saturated sodium bicarbonate solution, dried over magnesium fulfate, and evaporated leaving 11.85 g (91% of theory) of product. The FAB m.s. showed a molecular ion peak at 491.

1. additionwas added
2. additionthe reaction was carefully added
3. customThe organic layer was separated
4. extractionthe aqueous layer was extracted with another 50 ml of dichloromethane
5. washThe combined organic layers were washed with 3×80 ml of saturated sodium bicarbonate solution
6. dry with materialdried over magnesium fulfate
7. customevaporated
8. customleaving 11.85 g (91% of theory) of product