HRID890423
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- -70 °C
PROCEDURE
实验过程
To a dry ice chilled solution of 1.66 g (5.35 mmol) 4-methyl-2-(4-trifluoromethyl-phenyl)-pyrimidine-5-carboxylic acid ethyl ester in 20 ml THF was dropped at −70° C. 12.35 ml (16.05 mmol) 1.2M DIBALH solution in toluene. The reaction mixture was stirred 1 h at −70° C. and after attaining RT the reaction was stirred for another 2 h at this temperature. A solution of 50 ml of 1N HCl was added dropwise, then the reaction mixture partitioned between ether and water. The ether solution was concentrated under reduced pressure to provide 1.42 g of pure [4-methyl-2-(4-trifluoromethyl-phenyl)-pyrimidin-5-yl]-methanol.
WORKUP
后处理
- customafter attaining RT
- stirringwas stirred for another 2 h at this temperature
- customthe reaction mixture partitioned between ether and water
- concentrationThe ether solution was concentrated under reduced pressure