反応 #968

反応方程式

3-cyanomethyl-1-benzhydryl azetidine

LiAlH4

hydride

→

title compound

収率 87.0%

3-aminoethyl-1-benzhydryl azetidine

収率 87.0%

溶媒

THF

反応条件

後処理

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

実験手順

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.

出典