Reaktion #78351

Reaktionsgleichung

4-amino-4-phenylpiperidine dibenzenesulfonate

compound

1-Benzoyl-3-(3,4-dichlorophenyl)-3-[3-[4-(pyrrolidin-1-ylcarbonyl)piperid-1-yl]propyl]piperidine Hydrochloride

K2CO3

→

expected product

Ausbeute 74.6%

3-[3-(4-Amino-4-phenylpiperid-1-yl)propyl]-1-benzoyl-3-(3,4-dichlorophenyl)-piperidine

Ausbeute 74.6%

Lösungsmittel

DMF acetonitrile

Reaktionsbedingungen

Aufarbeitung

1. 1
   EinengenIt is concentrated under vacuum
2. 2
   Extraktionextracted with AcOEt
3. 3
   Waschenthe organic phase is washed with water and with saturated NaCl solution
4. 4
   Trocknendried over MgSO4
5. 5
   Sonstigethe solvent is evaporated off under vacuum
6. 6
   SonstigeThe residue is chromatographed on silica H

Vorschrift

A mixture of 6.81 g of 4-amino-4-phenylpiperidine dibenzenesulfonate, 5.2 g of the compound obtained in step B of EXAMPLE 1 and 6.1 g of K2CO3 in 30 ml of a DMF/acetonitrile mixture (50/50; v/v) is heated at 100° C. for 5 hours. It is concentrated under vacuum, the residue is taken up with water and extracted with AcOEt, the organic phase is washed with water and with saturated NaCl solution and dried over MgSO4 and the solvent is evaporated off under vacuum. The residue is chromatographed on silica H using a DCM/MeOH mixture (from 99/1; v/v to 85/15; v/v) as the eluent to give 3.6 g of the expected product.

Quelle