反应 #968

反应方程式

3-cyanomethyl-1-benzhydryl azetidine

LiAlH4

hydride

→

title compound

收率 87.0%

3-aminoethyl-1-benzhydryl azetidine

收率 87.0%

溶剂

THF

反应条件

后处理

1. 1
   温度The reaction mixture was refluxed for 4 h
2. 2
   过滤the gelatinous mixture was filtered
3. 3
   洗涤the filter cake was washed repeatedly with THF
4. 4
   其他The solvent was evaporated
5. 5
   workup.DISSOLUTIONthe residue was dissolved in diethyl ether
6. 6
   洗涤washed with brine
7. 7
   干燥dried with Na2SO4
8. 8
   其他Evaporation of the solvent

实验过程

5.7 g (21.7 mmol) of 3-cyanomethyl-1-benzhydryl azetidine was added slowly to a suspension of 2.9 g (76.0 mmol) of LiAlH4 in 80 mL of dry THF at roomtemperature. The reaction mixture was refluxed for 4 h. Excess hydride reagent was hydrolyzed by careful addition, with cooling, of NH4 Cl(aq), the gelatinous mixture was filtered and the filter cake was washed repeatedly with THF. The solvent was evaporated, the residue was dissolved in diethyl ether, washed with brine and dried with Na2SO4. Evaporation of the solvent gave 5.0 g (87%) of the title compound.

来源