反应 #55626

反应方程式

N-benzyloxycarbonyloxysuccinimide

water

γ-aminobutyric acid

sodium bicarbonate

→

N-carbobenzoxy-γ-aminobutyric acid

溶剂

tetrahydrofuran

反应条件

后处理

1. 1
   其他the tetrahydrofuran is evaporated in vacuo
2. 2
   workup.ADDITIONThe residue is diluted with 200 ml
3. 3
   萃取of water and extracted with (2×300 ml.) anhydrous ether
4. 4
   萃取extracted with (3×400 ml.) methylene chloride
5. 5
   其他The methylene chloride extracts are collected
6. 6
   洗涤washed with (3×200 ml.) brine solution
7. 7
   干燥dried with anhydrous magnesium sulfate
8. 8
   其他the solvent evaporated in vacuo at room temperature

实验过程

To a solution of 100 ml. of water and 120 ml. of tetrahydrofuran is added sequentially 12.4 g. of γ-aminobutyric acid, 10.4 g. of sodium bicarbonate, and 30 g. of N-benzyloxycarbonyloxysuccinimide. The reaction mixture is stirred for approximately 3.5 hours at room temperature and then the tetrahydrofuran is evaporated in vacuo. The residue is diluted with 200 ml. of water and extracted with (2×300 ml.) anhydrous ether. The aqueous layer is then acidified to pH 1-2 with 1 N hydrochloric acid and extracted with (3×400 ml.) methylene chloride. The methylene chloride extracts are collected and combined and then washed with (3×200 ml.) brine solution, dried with anhydrous magnesium sulfate and the solvent evaporated in vacuo at room temperature. The residue provides N-carbobenzoxy-γ-aminobutyric acid.

来源