반응 #78349

반응 방정식

hydrogen chloride

4-(2-hydroxyethoxy)-4-phenylpiperidine hydrochloride

compound

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

K2CO3

→

expected product

수율 128.8%

1-Benzoyl-3-(3,4-dichlorophenyl)-3-[3-[4-(2-hydroxyethoxy)-4-phenyl-piperid-1-yl]propyl]piperidine Hydrochloride Monohydrate

수율 128.8%

용매

DCM

water

DMF

반응 조건

후처리

1. 1
   추출extracted with DCM
2. 2
   세척the organic phase is washed with water
3. 3
   건조dried over Na2SO4
4. 4
   기타the solvent is evaporated off under vacuum
5. 5
   기타The residue is chromatographed on silica H
6. 6
   기타The product obtained
7. 7
   기타the precipitate formed
8. 8
   여과is filtered off

실험 절차

A mixture of 1 g of 4-(2-hydroxyethoxy)-4-phenylpiperidine hydrochloride, 1.7 g of the compound obtained in step B of EXAMPLE 1 and 0.65 g of K2CO3 in 15 ml of DMF is heated at 60° C. for 2 hours and the reaction mixture is then stirred overnight at RT. It is poured into water and extracted with DCM, the organic phase is washed with water and dried over Na2SO4 and the solvent is evaporated off under vacuum. The residue is chromatographed on silica H using DCM and then a DCM/MeOH mixture (96/4; v/v) as the eluent. The product obtained is dissolved in DCM and acidified by the addition of ethereal hydrogen chloride and the precipitate formed is filtered off to give 1.2 g of the expected product, m.p.=120-123° C.

출처