반응 #366475

ord-5d4248cec91a4c448519730ebdb6bc0a

용매

반응 조건

온도
60°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도cooled to 25° C.
  2. 2
    농축concentrated
  3. 3
    기타The residue was partitioned between CH2Cl2 (75 mL) and water (50 mL)
  4. 4
    세척was washed with water (2×50 mL) and brine (1×50 mL)
  5. 5
    건조The organic phase was dried (MgSO4)
  6. 6
    농축concentrated

실험 절차

A solution of 4-(aminomethyl)piperidine (7.00 g, 61.3 mmol) in CH3CN (100 mL) was treated sequentially with K2CO3 (3.02 g) and 4-chlorobenzyl chloride (3.52 g, 21.8 mmol). The reaction mixture was heated to 60° C. for 16 h, cooled to 25° C. and concentrated. The residue was partitioned between CH2Cl2 (75 mL) and water (50 mL), and was washed with water (2×50 mL) and brine (1×50 mL). The organic phase was dried (MgSO4) and concentrated. Chromatography (SiO2, 4% H2O-iPrOH) afforded4-(aminomethyl)-1-(4-chlorobenzyl)piperidine (3.58 g, 69%).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US06362177B1uspto-grants-2002_03