반응 #671231

ord-83300e617b1e43b39110562d9603024c

반응 방정식

CC#N
CH3CN
FC(F)(F)c1cc(Cl)cc(N2CCNCC2)c1
1-(3-Chloro-5-trifluoromethyl-phenyl)-piperazine
O=C([O-])[O-].[K+].[K+]
K2CO3
CC#N
CH3CN
CCCN1CCN(c2cc(Cl)cc(C(F)(F)F)c2)CC1
title compound
CCCN1CCN(c2cc(Cl)cc(C(F)(F)F)c2)CC1
1-(3-Chloro-5-trifluoromethyl-phenyl)-4-propyl-piperazine

반응 조건

온도
50°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    여과The reaction mixture was filtered
  2. 2
    기타the volatiles were evaporated in vacuum
  3. 3
    기타The oily residue was chromatographed on a silica column with MeOH: CH2Cl2 (1:9 (v/v)) as eluent
  4. 4
    기타Collection of the fractions
  5. 5
    workup.ADDITIONcontaining pure
  6. 6
    기타product and evaporation of the solvent

실험 절차

A suspension of 1-(3-Chloro-5-trifluoromethyl-phenyl)-piperazine (100 mg) and ground K2CO3 (200 mg) was stirred in CH3CN (30 mL) at room temperature. A solution of 1-bromo-propyl (52 mg) in CH3CN (5 mL) was added dropwise. The mixture was stirred at 50° C. overnight. The reaction mixture was filtered and the volatiles were evaporated in vacuum. The oily residue was chromatographed on a silica column with MeOH: CH2Cl2 (1:9 (v/v)) as eluent. Collection of the fractions containing pure product and evaporation of the solvent afforded the title compound (85 mg). MS m/z (relative intensity, 70 eV) 306 (M+, 25), 277 (bp), 234 (23), 206 (23), 179 (23).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US06924374B2uspto-grants-2005_08