反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperaturethe mixture was cooled to 5° C.
- filtrationfiltered
- customdried