HRID1697892

反应详情

EQUATION

反应方程式

HRID 1697892 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

21% Sodium ethoxide in ethanol (21:79, sodium ethoxide:ethanol, 56.0 mL) was added dropwise to a mixture of ethyl-beta-benzylaminopropionate (22.178 g, 0.10700 mol) and diethyl oxalate (15.0 mL, 0.110 mol). The reaction mixture was stirred at room temperature for 1 hour. The reaction mixture was concentrated and then water (about 200 mL) was added. The mixture was stirred for 5 min and then 1M HCl was added until pH 1. The mixture was vacuum filtered. The solids were collected and dried in vacuo overnight, and then crystallized from ethanol to give the desired product (20.946 g, 75%).

WORKUP

后处理

  1. concentrationThe reaction mixture was concentrated
  2. additionwater (about 200 mL) was added
  3. stirringThe mixture was stirred for 5 min
  4. addition1M HCl was added until pH 1
  5. filtrationfiltered
  6. customThe solids were collected
  7. customdried in vacuo overnight
  8. customcrystallized from ethanol