HRID2185666

反应详情

EQUATION

反应方程式

HRID 2185666 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

7.699 g (25.9 mmol) of N-benzyloxycarbonyl-2(S)-indolinecarboxylic acid prepared as in Example 16 a) are dissolved in tetrahydrofuran (150 ml), under nitrogen. 2.986 g (25.9 mmol) of N-ethylmorpholine are added, at 0° C., followed by 3.54 g (25.9 mmol) of isobutyl chloroformate. After 45 minutes, 1.903 g (25.9 mmol) of n-butylamine are added and the suspension is stirred overnight. Methylene chloride (300 ml) is added and the organic phase is washed with 10% citric acid (3×100 ml) and then NaHCO3 (3×100 ml). After drying and evaporation, a white solid is obtained which is recrystallized from methanol.

WORKUP

后处理

  1. washthe organic phase is washed with 10% citric acid (3×100 ml)
  2. customAfter drying
  3. customevaporation
  4. customa white solid is obtained which
  5. customis recrystallized from methanol