반응 #968

반응 방정식

3-cyanomethyl-1-benzhydryl azetidine

LiAlH4

hydride

→

title compound

수율 87.0%

3-aminoethyl-1-benzhydryl azetidine

수율 87.0%

용매

THF

반응 조건

후처리

1. 1
   온도The reaction mixture was refluxed for 4 h
2. 2
   여과the gelatinous mixture was filtered
3. 3
   세척the filter cake was washed repeatedly with THF
4. 4
   기타The solvent was evaporated
5. 5
   workup.DISSOLUTIONthe residue was dissolved in diethyl ether
6. 6
   세척washed with brine
7. 7
   건조dried with Na2SO4
8. 8
   기타Evaporation of the solvent

실험 절차

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.

출처