HRID968471
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
CONDITIONS
反应条件
- 温度
- 50 °C
PROCEDURE
实验过程
9.6 g of propyl isocyanate were added to a solution of 50 g of enantiopure ethyl 3-{[(allyloxy)-carbonyl]-amino}-3-{{3-{[(3-aminophenyl)-sulfonyl]-amino}-phenyl}}-propanoate from fraction 1 from Example II.2.f in 500 ml of dioxane, and the mixture was stirred for 18 h at 50° C. After evaporation of the solvent, 1.5 L of 1 M hydrochloric acid were added, and the solution was extracted with dichloromethane. The organic phase was dried over magnesium sulphate and concentrated. Chromatography on silica gel (dichloromethane/methanol=30:1) yielded 19.1 g of the compound.
WORKUP
后处理
- customAfter evaporation of the solvent, 1.5 L of 1 M hydrochloric acid
- additionwere added
- extractionthe solution was extracted with dichloromethane
- dry with materialThe organic phase was dried over magnesium sulphate
- concentrationconcentrated