HRID1925774

反应详情

EQUATION

反应方程式

HRID 1925774 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

First, 20.0 g (0.124 mol) of L-glutamic acid-γ-methyl ester was suspended in 20 g of methanol. To this, 13.7 g (0.137 mol) of acetylacetone and 12.5 g (0.124 mol) of triethylamine were added. The mixture was stirred at 60° C. for one hour. Subsequently, 80 g (1.24 mol) of 70% ethylamine was added to the mixture. After the mixture was allowed to react for 6 hours, excessive ethylamine was distilled away under reduced pressure. To this, 11.4 g (0.246 mol) of formic acid and 120 mL of 2-propanol (IPA) were added. The crystal precipitated was filtrated by suction and washed with 20 mL of IPA to obtain wet matter. The wet matter was dried under reduced pressure to obtain 17.7 g of theanine as a white crystal substance (yield: 82%).

WORKUP

后处理

  1. customto react for 6 hours
  2. distillationexcessive ethylamine was distilled away under reduced pressure
  3. customThe crystal precipitated
  4. filtrationwas filtrated by suction
  5. washwashed with 20 mL of IPA
  6. customto obtain wet matter
  7. customThe wet matter was dried under reduced pressure