HRID2044025
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
- 35 °C
PROCEDURE
实验过程
The mixture of ethyl (3E)-3-(2,2-dimethyl-1,3-dioxolan-4-ylidene)-2-oxopropanoate (21.4 g, 0.1 mol) and 2-hydrazino-3-chloropyridine (14.3 g, 0.1 mol) in 50 ml of ethanol was stirred for 18 hours at 35° C. Ethanol was removed in vacuo and the residue was taken up in 100 ml of methyl (tert)-butyl ether. The organic phase was washed once with 50 ml of 1% strength HCl and concentrated by evaporation. This gave 26.2 g (86% yield) of the product as a viscous oil with a purity (HPLC) of 97%.
WORKUP
后处理
- customEthanol was removed in vacuo
- washThe organic phase was washed once with 50 ml of 1% strength HCl
- concentrationconcentrated by evaporation