HRID2064166

反应详情

EQUATION

反应方程式

HRID 2064166 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

1,1-Dimethylethyl 4-[(4-trifluoromethyl-5-chloro-2-nitrophenyl)amino]-1-piperidinecarboxylate (D61, 6.7 g) was dissolved in ethanol (100 ml) and Raney nickel (50% aqueous suspension, 5 ml) was added at room temperature; the mixture was heated to 50° C. and hydrazine monohydrate (3 ml) was added over 30 min. After 1 h more, the reaction mixture was cooled to room temperature, filtered through Celite, evaporated, re-evaporated from toluene, and the residue crystallised from dichloromethane to yield the subtitle compound, 4.0 g.

WORKUP

后处理

  1. temperaturethe reaction mixture was cooled to room temperature
  2. filtrationfiltered through Celite
  3. customevaporated
  4. customre-evaporated from toluene
  5. customthe residue crystallised from dichloromethane