Реакция #2320076

ord-69c44f30341648dc860a611521cb123d

Уравнение реакции

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

Условия реакции

Температура
50°CELSIUS
Подробные условия
See reaction.notes.procedure_details.

Обработка

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

Методика

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).

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: USRE041315E1uspto-grants-2010_05