반응 #78337

반응 방정식

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

용매

AcOEt

DMF acetonitrile

반응 조건

후처리

1. 1
   추출extracted with AcOEt
2. 2
   세척the organic phase is washed twice with water and with saturated NaCl solution
3. 3
   건조dried over MgSO4
4. 4
   기타the solvent is evaporated off under vacuum
5. 5
   기타The residue is chromatographed on silica H
6. 6
   기타The product obtained
7. 7
   기타a 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
   여과This gives 0.53 g of the expected product after filtration
10. 10
    기타drying

실험 절차

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.).

출처