تفاعل #78338

معادلة التفاعل

hydrogen chloride

4-(acryloyl-N-methylamino)-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 80.5%

3-[3-[4-(Acryloyl-N-methylamino)-4-phenylpiperid-1-yl]propyl]-1-benzoyl-3-(3,4-dichlorophenyl)piperidine Hydrochloride

المردود 80.5%

المذيبات

DCM

water

DMF

ظروف التفاعل

المعالجة

1. 1
   استخلاصextracted with AcOEt
2. 2
   غسيلthe organic phase is washed with water and with saturated NaCl solution
3. 3
   تجفيفdried over MgSO4
4. 4
   أخرىthe solvent is evaporated off under vacuum
5. 5
   أخرىThe residue is chromatographed on silica using a gradient of a DCM/MeOH mixture (99/1; v/v to 95/5; v/v) as the eluent
6. 6
   أخرىThe product obtained
7. 7
   أخرىthe precipitate formed
8. 8
   ترشيحis filtered off

الإجراء التجريبي

A mixture of 0.27 g of 4-(acryloyl-N-methylamino)-4-phenylpiperidine hydrochloride, 0.45 g of the compound obtained in step B of EXAMPLE 1 and 0.3 g of K2CO3 in 3 ml of DMF is heated at 80° C. for 2 hours. The reaction mixture is poured into water and extracted with AcOEt, the organic phase is washed with water and with saturated NaCl solution and dried over MgSO4 and the solvent is evaporated off under vacuum. The residue is chromatographed on silica using a gradient of a DCM/MeOH mixture (99/1; v/v to 95/5; 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 0.2 g of the expected product, m.p.=128° C.

المصدر