تفاعل #968

معادلة التفاعل

3-cyanomethyl-1-benzhydryl azetidine

LiAlH4

hydride

→

title compound

المردود 87.0%

3-aminoethyl-1-benzhydryl azetidine

المردود 87.0%

المذيبات

THF

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةThe reaction mixture was refluxed for 4 h
2. 2
   ترشيحthe gelatinous mixture was filtered
3. 3
   غسيلthe filter cake was washed repeatedly with THF
4. 4
   أخرىThe solvent was evaporated
5. 5
   workup.DISSOLUTIONthe residue was dissolved in diethyl ether
6. 6
   غسيلwashed with brine
7. 7
   تجفيفdried with Na2SO4
8. 8
   أخرىEvaporation of the solvent

الإجراء التجريبي

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.

المصدر