HRID233743
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
A solution of 0.73 g (3 mmol) of the compound from Example VI in 5 ml of ethyl acetate is added at 0° C. to a solution of 0.93 g (2.16 mmol) of (S)-isoleucine methyl ester isocyanate (prepared by reacting (S)-isoleucine methyl ester hydrochloride with trichloromethyl chloroformate in toluene at 120° C.) in 10 ml of ethyl acetate, and the mixture is stirred at this temperature for 30 min. Subsequently, the reaction mixture is washed successively with dilute hydrochloric acid, water and saturated solutions of sodium hydrogen carbonate and sodium chloride, and the organic phase is then concentrated and the residue purified on silica gel using petroleum ether/ethyl acetate (2:1).
WORKUP
后处理
- washSubsequently, the reaction mixture is washed successively with dilute hydrochloric acid, water and saturated solutions of sodium hydrogen carbonate and sodium chloride
- concentrationthe organic phase is then concentrated
- customthe residue purified on silica gel