HRID2064201

反应详情

EQUATION

反应方程式

HRID 2064201 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 1-benzyl-3-carbethoxy-4-piperidone (3 mmol, 784 mg) in xylene (20 mL) was treated at room temperature with 4,5-dimethyl-1,2-benzenediamine (3 mmol, 408.6 mg, 1 eq) and the suspension was stirred under reflux under argon overnight then further for 5 h. The mixture was concentrated under reduced pressure to give a brown residue, which was treated with ethyl acetate and a touch of methanol. Beige crystals formed from the brown solution and were filtered off and dried under reduced pressure (vacuum oven) to give the title compound (1.05 mmol, 350 mg, 35% yield). M+H 334.3.

WORKUP

后处理

  1. temperatureunder reflux under argon overnight
  2. concentrationThe mixture was concentrated under reduced pressure
  3. customto give a brown residue, which
  4. customBeige crystals formed from the brown solution
  5. filtrationwere filtered off
  6. customdried under reduced pressure (vacuum oven)