反応 #78337

反応方程式

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

溶媒

AcOEt

DMF acetonitrile

反応条件

後処理

1. 1
   抽出extracted with AcOEt
2. 2
   洗浄the organic phase is washed twice with water and with saturated NaCl solution
3. 3
   乾燥dried over MgSO4
4. 4
   その他the solvent is evaporated off under vacuum
5. 5
   その他The residue is chromatographed on silica H
6. 6
   その他The product obtained
7. 7
   その他a 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
   ろ過This gives 0.53 g of the expected product after filtration
10. 10
    その他drying

実験手順

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.).

出典