HRID130576

反应详情

EQUATION

反应方程式

HRID 130576 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. customequipped with a mechanical stirrer
  2. additionis added over a period of 15 minutes
  3. waitThe reaction mixture is left under agitation for 1 hour at 25° C.
  4. customThe solid obtained
  5. filtrationis filtered off
  6. washwashed with methanol
  7. customdried under vacuum