HRID269018

反应详情

EQUATION

反应方程式

HRID 269018 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
23 °C

PROCEDURE

实验过程

To a solution of 3-trifluoromethyl-pyridin-2-ylamine (16.21 g, 100 mmol) in acetonitrile (300 mL) at 5° C. was added NBS (17.8 g, 100 mmol) and the mixture was stirred at 23° C. for 1 h. Poured onto ice and sat. NaHCO3 soln., extracted with EtOAc, washed with brine, dried over Na2SO4. Removal of the solvent in vacuum left a yellow solid. Silica gel & cotton wool column filtratation with DCM gave the product as a yellow solid (23.71 g, 98%). MS (ISP) 240.1 [(M+H)+].

WORKUP

后处理

  1. extraction, extracted with EtOAc
  2. washwashed with brine
  3. dry with materialdried over Na2SO4
  4. customRemoval of the solvent in vacuum
  5. waitleft a yellow solid