HRID734769
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
- 0 °C
PROCEDURE
实验过程
3.00 g (79.36 mmol) of sodium borohydride was added batchwise to a solution of 14.48 g (52.91 mmol) of 1-benzyl-4-trifluoromethylpyridinium chloride in 100 mL of EtOH with strong cooling at 0° C., then the cooling was stopped and the reaction mixture was stirred for 1.5 hours at 14° C. While cooling, 50 mL of water and then 50 mL of EtOH were added within 30 minutes. The reaction mixture was stirred for another 30 minutes, the resulting suspension was filtered and the filtrate was evaporated down in vacuo. Yield: 11.72 g (92% of theoretical); C13H14F3N (M=241.252); calc.: molpeak (M+H)+: 242; found: molpeak (M+H)+: 242; HPLC-MS: 3.60 minutes (method B).
WORKUP
后处理
- temperatureWhile cooling
- stirringThe reaction mixture was stirred for another 30 minutes
- filtrationthe resulting suspension was filtered
- customthe filtrate was evaporated down in vacuo
- custom3.60 minutes (method B)