تفاعل #78337

معادلة التفاعل

water

4-piperidinopiperidine

compound

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

K2CO3

→

1-Benzoyl-3-(3,4-dichlorophenyl)-3-[3-(4-piperidinopiperid-1-yl)propyl]-piperidine Dihydrochloride Hemihydrate

المذيبات

AcOEt

DMF acetonitrile

ظروف التفاعل

المعالجة

1. 1
   استخلاصextracted with AcOEt
2. 2
   غسيلthe organic phase is washed twice 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 H
6. 6
   أخرىThe product obtained
7. 7
   أخرىa stream of HCl gas is bubbled into the solution until the pH is 1, and ether
8. 8
   workup.ADDITIONis added until precipitation
9. 9
   ترشيحThis gives 0.53 g of the expected product after filtration
10. 10
    أخرىdrying

الإجراء التجريبي

A mixture of 0.55 g of 4-piperidinopiperidine, 1.3 g of the compound obtained in step B of EXAMPLE 1 and 1.14 g of K2CO3 in 10 ml of a DMF/acetonitrile mixture (50/50; v/v) is heated at 100° C. for 3 hours. The reaction mixture is poured into water and extracted with AcOEt, the organic phase is washed twice 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 H using DCM and then a DCM/MeOH mixture (98/2; v/v) as the eluent. The product obtained is dissolved in AcOEt, a stream of HCl gas is bubbled into the solution until the pH is 1, and ether is added until precipitation occurs. This gives 0.53 g of the expected product after filtration and drying, m.p.=265° C. (dec.).

المصدر