HRID2275757

反应详情

EQUATION

反应方程式

HRID 2275757 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

130 g of 3-(cyclohexylmethoxy)pyridine-2-amine (Example 4A; 630 mmol, 1 equivalent) were initially charged in 3950 ml of ethanol, and 436 ml of ethyl 2-chloroacetoacetate (3.2 mol, 5 equivalents) were added. The mixture was heated under reflux for 24 h and then concentrated under reduced pressure. The crude product obtained in this manner was chromatographed on silica gel using cyclohexane/diethyl ether as mobile phase, giving 66.2 g (33% of theory) of the title compound.

WORKUP

后处理

  1. temperatureThe mixture was heated
  2. temperatureunder reflux for 24 h
  3. concentrationconcentrated under reduced pressure
  4. customThe crude product obtained in this manner
  5. customwas chromatographed on silica gel