Reacción #78349

Ecuación de reacción

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

Rendimiento 128.8%

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

Rendimiento 128.8%

Disolventes

DCM

water

DMF

Condiciones de reacción

Tratamiento posterior

1. 1
   Extracciónextracted with DCM
2. 2
   Lavadothe organic phase is washed with water
3. 3
   Secadodried over Na2SO4
4. 4
   Otrothe solvent is evaporated off under vacuum
5. 5
   OtroThe residue is chromatographed on silica H
6. 6
   OtroThe product obtained
7. 7
   Otrothe precipitate formed
8. 8
   Filtraciónis filtered off

Procedimiento

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.

Fuente