HRID968471

反应详情

EQUATION

反应方程式

HRID 968471 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. customAfter evaporation of the solvent, 1.5 L of 1 M hydrochloric acid
  2. additionwere added
  3. extractionthe solution was extracted with dichloromethane
  4. dry with materialThe organic phase was dried over magnesium sulphate
  5. concentrationconcentrated