HRID1941337

反应详情

EQUATION

反应方程式

HRID 1941337 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of N-butanesulfonyl-N-trimethylsilylamide (0.75 g, 3.6 mmol), t-butoxycarbonyltryptophan fluoride (0.92 g, 3.01 mmol), and dimethylaminopyridine (37 mg, 0.3 mmol) in tetrahydrofuran (10 ml) is stirred at room temperature for 2 hours. The mixture is diluted with 10% citric acid and extracted with ethyl acetate. The organic layer is washed with water and brine, dried over magnesium sulfate, and concentrated in vacuo. The crude material is chromatographed on silica gel with ethyl acetate/hexane (1:1) and trace of acetic acid to give N-butanesulfonyl-(t-butoxycarbonyl)tryptophanamide.

WORKUP

后处理

  1. extractionextracted with ethyl acetate
  2. washThe organic layer is washed with water and brine
  3. dry with materialdried over magnesium sulfate
  4. concentrationconcentrated in vacuo
  5. customThe crude material is chromatographed on silica gel with ethyl acetate/hexane (1:1) and trace of acetic acid