HRID130400

反应详情

EQUATION

反应方程式

HRID 130400 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of cis-3,5-dimethyl-1-[4-(methyloxy)-3-nitrophenyl]piperazine (D3) (2.65 g, 10 mmol) in ethanol (60 ml) containing palladium on charcoal (300 mg, 10% paste) was stirred under aone atmosphere of hydrogen gas overnight. The mixture was filtered through celite, the pad washed in ethanol and the combined ethanol solutions evaporated. The residue was purified by column chromatography (Biotage (SiO2) 100 g, dichloromethane to 1:10 2M ammonia in methanol:dichloromethane) to afford the title product (D4). MS (ES+) m/e 236 [M+H]+.

WORKUP

后处理

  1. filtrationThe mixture was filtered through celite
  2. washthe pad washed in ethanol
  3. customthe combined ethanol solutions evaporated
  4. customThe residue was purified by column chromatography (Biotage (SiO2) 100 g, dichloromethane to 1:10 2M ammonia in methanol:dichloromethane)