HRID1058096
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customthe resulting reaction mixture
- waitAfter 0.5 hours
- stirringstirred at 0° C
- waitAfter 8 h
- filtrationthe white precipitate was filtered off
- customdried at 40° C.