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
PROCEDURE
实验过程
To a suspension of [4-azido-2-(trifluoromethyl)phenyl](2-pyridyl)methanone (2.0 g) in THF (20 ml) was added dropwise a solution of aluminum lithium hydride (520 mg) in. THF (20 ml) at 0° C. under nitrogen atmosphere. After finishing the dropping, the mixture was allowed to be at room temperature, and the mixture was stirred for 1 hour. Water (0.52 ml), 15% aqueous solution of sodium hydroxide (0.52 ml) and water (1.6 ml) were sequentially added to the mixture at 0° C., and the mixture was allowed to be at room temperature and the mixture was stirred overnight. Magnesium sulfate was added to the mixture, and the unnecessary substances were filtered off. The solvent was distilled off under reduced pressure and the obtained residue was recrystallized from hexane-ethyl acetate, to give [4-amino-2-(trifluoromethyl)phenyl](2-pyridyl)methanol (1.51 g) as colorless crystals.
WORKUP
后处理
- customat 0° C.
- customto be at room temperature
- customto be at room temperature
- stirringthe mixture was stirred overnight
- filtrationthe unnecessary substances were filtered off
- distillationThe solvent was distilled off under reduced pressure
- customthe obtained residue was recrystallized from hexane-ethyl acetate