HRID1515371
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
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 (21.4 g, 0.15 mol) in 150 ml of ethanol was stirred for 8 hours at RT. Ethanol was removed in vacuo and the residue was taken up in 200 ml of methyl tert-butyl ethyl. The organic phase was washed three times with in each case 50 ml of 1% HCl and concentrated by evaporation. This gave 36 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 three times with in each case 50 ml of 1% HCl
- concentrationconcentrated by evaporation