반응 #220768

반응 방정식

K2CO3

4-chlorobenzyl chloride

4-(aminomethyl)piperidine

→

4-(aminomethyl)-1-(4-chlorobenzyl)piperidine

수율 69.0%

용매

acetonitrile

반응 조건

후처리

1. 1
   기타The resulting reaction mixture
2. 2
   온도cooled to 25° C.
3. 3
   농축concentrated
4. 4
   세척washed with water (50 mL×2) and brine (50 mL×1)
5. 5
   건조The organic layer was dried (over MgSO4)
6. 6
   농축concentrated
7. 7
   기타purified by chromatography (SiO2, 4% H2O-iPrOH)

실험 절차

K2CO3 (3.02 g) and 4-chlorobenzyl chloride (3.52 g, 21.8 mmol) were successively added to an acetonitrile (100 mL) solution of 4-(aminomethyl)piperidine (7.00 g, 61.3 mmol). The resulting reaction mixture was stirred at 60° C. for 16 hours, cooled to 25° C. and concentrated. The obtained residue was fractionated between dichloromethane (75 mL) and water (50 mL) and then washed with water (50 mL×2) and brine (50 mL×1). The organic layer was dried (over MgSO4), concentrated and then purified by chromatography (SiO2, 4% H2O-iPrOH) to provide 4-(aminomethyl)-1-(4-chlorobenzyl)piperidine (3.58 g, 69%).

출처