반응 #78351

반응 방정식

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

수율 74.6%

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

수율 74.6%

용매

DMF acetonitrile

반응 조건

후처리

1. 1
   농축It is concentrated under vacuum
2. 2
   추출extracted with AcOEt
3. 3
   세척the organic phase is washed with water and with saturated NaCl solution
4. 4
   건조dried over MgSO4
5. 5
   기타the solvent is evaporated off under vacuum
6. 6
   기타The residue is chromatographed on silica H

실험 절차

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.

출처