HRID1486031

反应详情

EQUATION

反应方程式

HRID 1486031 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of (2S,3S)-2-tert-butoxycarbonylamino-3-(2-nitro-phenylamino)-butyric acid methyl ester (5.71 g, 16.2 mmol) in dioxane water (1:1, 100 ml) was added an aqueous solution of 2.5 M lithium hydroxide (31 ml) and the reaction was stirred at ambient temperature for 2 h. The reaction was made acidic with 10% aqueous citric acid, diluted with water (60 ml) and extracted with ethyl acetate (2×100 mL). The organic layers were combined, washed with water (1×50 mL), brine, dried over sodium sulfate, filtered and concentrated in vacuo to give (2S,3S)-2-tert-butoxycarbonylamino-3-(2-nitro-phenylamino)-butyric acid which was carried to the subsequent step without purification (5.48 g, 99%).

WORKUP

后处理

  1. extractionextracted with ethyl acetate (2×100 mL)
  2. washwashed with water (1×50 mL), brine
  3. dry with materialdried over sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo