HRID2064159

反应详情

EQUATION

反应方程式

HRID 2064159 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
45 °C

PROCEDURE

实验过程

A stirred suspension of N-[5-bromo-2-nitro-4-(trifluoromethyl)phenyl]-1-(tetrahydro-2H-pyran-4-yl)-4-piperidinamine (D54) (380 mg, 0.84 mmole) in ethanol (20 ml) at room temperature under argon was treated with Raney Nickel (20 mg) followed by the dropwise addition of hydrazine hydrate (0.25 ml, 8.0 mmole). The mixture was maintained at room temp. for 0.5 hr, then heated at 45° C. for 1 hr producing a grey solution, which was filtered through Kieselguhr and the filtrate concentrated under vacuum to afford the title compound as a pale yellow solid (350 mg, 99%). MH+=422, 424.

WORKUP

后处理

  1. temperatureThe mixture was maintained at room temp. for 0.5 hr
  2. customproducing a grey solution, which
  3. filtrationwas filtered through Kieselguhr
  4. concentrationthe filtrate concentrated under vacuum