تفاعل #78349

معادلة التفاعل

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

المردود 128.8%

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

المردود 128.8%

المذيبات

DCM

water

DMF

ظروف التفاعل

المعالجة

1. 1
   استخلاصextracted with DCM
2. 2
   غسيلthe organic phase is washed with water
3. 3
   تجفيفdried over Na2SO4
4. 4
   أخرىthe solvent is evaporated off under vacuum
5. 5
   أخرىThe residue is chromatographed on silica H
6. 6
   أخرىThe product obtained
7. 7
   أخرىthe precipitate formed
8. 8
   ترشيحis filtered off

الإجراء التجريبي

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.

المصدر