反応 #78349

反応方程式

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

収率 128.8%

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

収率 128.8%

溶媒

DCM

water

DMF

反応条件

後処理

1. 1
   抽出extracted with DCM
2. 2
   洗浄the organic phase is washed with water
3. 3
   乾燥dried over Na2SO4
4. 4
   その他the solvent is evaporated off under vacuum
5. 5
   その他The residue is chromatographed on silica H
6. 6
   その他The product obtained
7. 7
   その他the precipitate formed
8. 8
   ろ過is filtered off

実験手順

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.

出典