HRID130576
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
24 ml of a 5.4 M solution of sodium methylate in methanol, 17.7 g of dimethylmalonate and 100 ml of methanol are placed in a 250 ml flask equipped with a mechanical stirrer, thermometer and condenser, under nitrogen flow. After 30 minutes, when the sodium has completely dissolved, a suspension of 20 g cyclohexylidenecyanoacetamide in 50 ml of methanol is added over a period of 15 minutes. The reaction mixture is left under agitation for 1 hour at 25° C. and is subsequently acidified with 5% HCl. The solid obtained is filtered off, washed with methanol and dried under vacuum. 28 g of methyl 5-cyano-2,4-dioxo-3-azaspiro[5,5]undecane-1-carboxylate are obtained.
WORKUP
后处理
- customequipped with a mechanical stirrer
- additionis added over a period of 15 minutes
- waitThe reaction mixture is left under agitation for 1 hour at 25° C.
- customThe solid obtained
- filtrationis filtered off
- washwashed with methanol
- customdried under vacuum