HRID336178

反应详情

EQUATION

反应方程式

HRID 336178 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
175 °C

PROCEDURE

实验过程

A microwave reaction vial is charged with piperidine-3-carboxylic acid (5-tert-butyl-isoxazol-3-yl)-amide; hydrochloride (94 mg; 0.327 mmol), 3-chloro-2-fluoro-5-trifluoromethylpyridine (0.043 mL; 0.33 mmol), triethylamine (0.092 mL; 0.66 mmol) and t-butanol (0.5 mL). The vial is heated in microwave at 175° C. for 1 hour then left standing at room temperature overnight. The reaction mixture is concentrated in vacuo. Purification by flash chromatography on silica using methanol/methylene chloride then recrystallization from hot methanol provides the title compound, m/z 431 [M+H+].

WORKUP

后处理

  1. customA microwave reaction
  2. waitthen left
  3. concentrationThe reaction mixture is concentrated in vacuo
  4. customPurification by flash chromatography on silica
  5. customrecrystallization from hot methanol