反応 #78345

反応方程式

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

溶媒

water

DMF

反応条件

後処理

1. 1
   その他the precipitate formed
2. 2
   ろ過is filtered off
3. 3
   洗浄washed with water
4. 4
   workup.DISSOLUTIONThe precipitate is dissolved in AcOEt
5. 5
   乾燥the organic phase is dried over MgSO4
6. 6
   その他the solvent is evaporated off under vacuum
7. 7
   その他The residue is chromatographed on silica H
8. 8
   その他The product obtained
9. 9
   その他the precipitate formed
10. 10
    ろ過is filtered off

実験手順

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.

出典