Reaktion #61047

ord-a069e09d936f4d85ab9ab67addd0230e

Reaktionsgleichung

CS(=O)(=O)c1ccc(I)c(C(=O)N2CCN(c3ccc(C(F)(F)F)cc3)CC2)c1
(2-Iodo-5-methanesulfonyl-phenyl)-[4-(4-trifluoromethyl-phenyl)-piperazin-1-yl]-methanone
NC1CCC1
cyclobutylamine
CS(=O)(=O)c1ccc(NC2CCC2)c(C(=O)N2CCN(c3ccc(C(F)(F)F)cc3)CC2)c1
title compound
Ausbeute 54.0%
CS(=O)(=O)c1ccc(NC2CCC2)c(C(=O)N2CCN(c3ccc(C(F)(F)F)cc3)CC2)c1
(2-Cyclobutylamino-5-methanesulfonyl-phenyl)-[4-(4-trifluoromethyl-phenyl)-piperazin-1-yl]-methanone
Ausbeute 54.0%

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Einengenbefore being concentrated in vacuo
  2. 2
    Waschenwashed with water
  3. 3
    Trocknendried over sodiumsulfate
  4. 4
    Filtrationfiltered
  5. 5
    Einengenconcentrated
  6. 6
    SonstigeThe residue was purified by column chromatography (SiO2, 5 g, Heptane/EtOAc 0-50%)

Vorschrift

A solution of (2-Iodo-5-methanesulfonyl-phenyl)-[4-(4-trifluoromethyl-phenyl)-piperazin-1-yl]-methanone (compound CK, 0.05 g, 0.09 mmol) and of cyclobutylamine (0.1 ml) in dimethylacetamide was heated in a microwave oven (180 deg) for 10 min before being concentrated in vacuo. The residue was disolve in ethyl acetate, washed with water dried over sodiumsulfate, filtered and concentrated. The residue was purified by column chromatography (SiO2, 5 g, Heptane/EtOAc 0-50%) to give the title compound as a white foam (24 mg, 54%). MS (m/e): 482.5 (M+H+, 100%).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07427612B2uspto-grants-2008_09