HRID1853945

反应详情

EQUATION

反应方程式

HRID 1853945 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-(2-Methyl-5-nitro-phenyl)-piperidin-4-one [100 mg, 0.426 mmol] in N,N-Dimethylformamide dimethyl acetal (DMA.DMF) [1 ml] was heated to reflux for 12 hrs. After cooling to room temperature, reaction mixture was concentrated under vacuum. The dark brown crude product obtained was further purified by silica gel chromatography using 30-60% ethyl acetate/hexane as eluent to obtain pure desired product i.e., 3-Dimethylaminomethylene-1-(2-methyl-5-nitro-phenyl)-piperidin-4-one [4] as orange solid [Yield: 76.2 mg, 62.02%]

WORKUP

后处理

  1. temperatureto reflux for 12 hrs
  2. customreaction mixture
  3. concentrationwas concentrated under vacuum
  4. customThe dark brown crude product obtained
  5. customwas further purified by silica gel chromatography