HRID639142

反应详情

EQUATION

反应方程式

HRID 639142 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

4

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

500 mg (5.88 mmol) Cyanoacetic acid are dissolved in 30 ml dimethylformamide, 563 mg (6.47 mmol) morpholine, 794 mg (5.88 mmol) 1-hydroxy-1H-benzotriazole hydrate and 718 mg (5.88 mmol) 4-dimethylaminopyridine are added. The reaction mixture is stirred at 0° C., then 1.12 g (5.88 mmol) 1-(3-dimethylaminopropyl)-3-ethylcarbodimide hydrochloride are added. The reaction mixture is stirred at room temperature for 18 hours, then water and ethyl acetate are added. The organic phase is dried over sodium sulfate and evaporated to dryness in vacuo. The residue is purified by preparative HPLC.

WORKUP

后处理

  1. stirringThe reaction mixture is stirred at room temperature for 18 hours
  2. dry with materialThe organic phase is dried over sodium sulfate
  3. customevaporated to dryness in vacuo
  4. customThe residue is purified by preparative HPLC