HRID582963

反应详情

EQUATION

反应方程式

HRID 582963 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
85 °C

PROCEDURE

实验过程

A 500 mL flask was charged with 5-benzyl-2-[4-hydroxyphenyl]pyrimidine (10.0 g, 40 mmol), 3-(2-(2-(nonafluorobutoxy)tetrafluoroethoxy)-2,2-difluoroethoxy)-1-bromopropane (24.2 g, 44 mmol, Example 3), potassium carbonate (6.1 g, 44 mmol), and anhydrous acetonitrile (100 mL), and the resulting mixture was stirred overnight at 85° C. under nitrogen. Water (150 mL) was added and the mixture was cooled to 5° C. and then filtered and dried to produce 5-benzyloxy-2-[4-(3-(2-(2-(nonafluorobutoxy)tetrafluoroethoxy)-2,2-difluoroethoxy)propoxy)phenyl]pyrimidine. This intermediate was further purified by recrystallization from acetone, and the benzyl protecting group was removed by hydrogenation using Pd/C catalyst.

WORKUP

后处理

  1. temperaturethe mixture was cooled to 5° C.
  2. filtrationfiltered
  3. customdried