HRID1058096

反应详情

EQUATION

反应方程式

HRID 1058096 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
-2.5 °C

PROCEDURE

实验过程

Glacial acetic acid (526.9 g, 8.78 mol) was added dropwise at <−5° C. to a suspension of methyl 3-amino-3-(3-pyridyl)-2-propenoate (0.45 mol) and sodium borohydride (44.3 g, 1.17 mol) in THF (500 g) and the resulting reaction mixture was stirred at −5-0° C. After 5 h, methanol (600 g) was added dropwise to the solution at −5-0° C. After 0.5 hours, HCl (163 g, 4.47 mol) was bubbled through the solution and stirred at 0° C. After 8 h, the white precipitate was filtered off and dried at 40° C. to yield 101.6 g (89%) of methyl 3-Amino-3-(3-pyridyl)propanoate dihydrochloride.

WORKUP

后处理

  1. customthe resulting reaction mixture
  2. waitAfter 0.5 hours
  3. stirringstirred at 0° C
  4. waitAfter 8 h
  5. filtrationthe white precipitate was filtered off
  6. customdried at 40° C.