HRID230945

反应详情

EQUATION

反应方程式

HRID 230945 的结构方程式

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

Combine a mixture of 2-chloro-4-(3-chloro-4-fluoro-phenyl)-6-[4-(3-trifluoromethyl-pyridin-2-yl)-piperazin-1-yl]-pyrimidine (47 mg, 1 mmol) and diethylamine (2 mL). Heat the mixture in a sealed tube at 60° C. for 16 hours. Cool to room temperature and evaporate. Add 1 M NaOH (1 mL) and extract 2× with EtOAc (2 mL each). Combine the organic layers, dry (Na2SO4), and purify using preparative TLC (9:1 hexanes/EtOAc) to obtain {4-(3-Chloro-4-fluoro-phenyl)-6-[4-(3-trifluoromethyl-pyridin-2-yl)-piperazin-1-yl]-pyrimidin-2-yl}-diethyl-amine as a white solid.

WORKUP

后处理

  1. temperatureCool to room temperature
  2. customevaporate
  3. additionAdd 1 M NaOH (1 mL)
  4. extractionextract 2× with EtOAc (2 mL each)
  5. dry with materialCombine the organic layers, dry (Na2SO4)
  6. custompurify