反応 #78351

反応方程式

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

収率 74.6%

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

収率 74.6%

溶媒

DMF acetonitrile

反応条件

後処理

1. 1
   濃縮It is concentrated under vacuum
2. 2
   抽出extracted with AcOEt
3. 3
   洗浄the organic phase is washed with water and with saturated NaCl solution
4. 4
   乾燥dried over MgSO4
5. 5
   その他the solvent is evaporated off under vacuum
6. 6
   その他The residue is chromatographed on silica H

実験手順

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.

出典