반응 #78345

반응 방정식

hydrogen chloride

4-benzyl-4-(pyrrolidin-1-ylcarbonyl)piperidine p-toluene-sulfonate

compound

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

K2CO3

→

expected product

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

용매

water

DMF

반응 조건

후처리

1. 1
   기타the precipitate formed
2. 2
   여과is filtered off
3. 3
   세척washed with water
4. 4
   workup.DISSOLUTIONThe precipitate is dissolved in AcOEt
5. 5
   건조the organic phase is dried over MgSO4
6. 6
   기타the solvent is evaporated off under vacuum
7. 7
   기타The residue is chromatographed on silica H
8. 8
   기타The product obtained
9. 9
   기타the precipitate formed
10. 10
    여과is filtered off

실험 절차

A mixture of 4-benzyl-4-(pyrrolidin-1-ylcarbonyl)piperidine p-toluene-sulfonate, 0.65 g of the compound obtained in step B of EXAMPLE 1 and 0.7 g of K2CO3 in 6 ml of DMF is heated at 80° C. for 3 hours. The reaction mixture is poured into iced water and the precipitate formed is filtered off and washed with water. The precipitate is dissolved in AcOEt, the organic phase is dried over MgSO4 and the solvent is evaporated off under vacuum. The residue is chromatographed on silica H using DCM and then a DCM/MeOH mixture (95/5; v/v) as the eluent. The product obtained is taken up with ethereal hydrogen chloride and the precipitate formed is filtered off to give 0.56 g of the expected product.

출처