Reaktion #11721

ord-03d958e6728f4420bdfbc1d54303f87c

Reaktionsgleichung

O=C(Cl)CCl
chloroacetyl chloride
C[C@@H]1CN(Cc2ccc(F)cc2)CCN1
(3R)-1-(4-fluoro-benzyl)-3-methyl-piperazine
CCN(CC)CC
triethylamine
C[C@@H]1CN(Cc2ccc(F)cc2)CCN1C(=O)CCl
title compound
C[C@@H]1CN(Cc2ccc(F)cc2)CCN1C(=O)CCl
2-Chloro-1-[4-(4-fluoro-benzyl)-(2R)-2-methyl-piperazin-1-yl]-ethanone

Reaktionsbedingungen

Temperatur
0°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturto warm to ambient temperature
  2. 2
    Waschenwashed with 10% citric acid
  3. 3
    SonstigeThe organic layer was separated
  4. 4
    Trocknendried over magnesium sulfate
  5. 5
    Filtrationfiltered
  6. 6
    Einengenconcentrated in vacuo

Vorschrift

To a solution of (3R)-1-(4-fluoro-benzyl)-3-methyl-piperazine (3 g, 14.4 mmol) in dichloromethane (40 mL) was added triethylamine (2.0 mL, 14.4 mmol). The reaction was cooled to 0° C. and chloroacetyl chloride was added (1.1 mL, 14.4 mmol). The reaction was allowed to warm to ambient temperature and stirred for 2 hours. The reaction is diluted with dichloromethane and washed with 10% citric acid. The organic layer was separated, dried over magnesium sulfate, filtered and concentrated in vacuo. Chromatography on silica gel gave the title compound (3.9 g).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07098212B2uspto-grants-2006_08