반응 #78350

반응 방정식

hydrogen chloride

compound

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

triethylamine

acetyl chloride

→

expected product

3-[3-[4-(2-Acetoxyethoxy)-4-phenylpiperid-1-yl]propyl]-1-benzoyl-3-(3,4-dichlorophenyl)piperidine Hydrochloride

용매

DCM

DCM

반응 조건

후처리

1. 1
   기타to rise to RT
2. 2
   농축It is concentrated under vacuum
3. 3
   추출extracted with AcOEt
4. 4
   세척the organic phase is washed with water
5. 5
   건조dried over Na2SO4
6. 6
   기타the solvent is evaporated off under vacuum
7. 7
   기타The residue is chromatographed on silica
8. 8
   기타The product obtained
9. 9
   기타the precipitate formed
10. 10
    여과is filtered off

실험 절차

A solution of 0.6 g of the compound obtained in EXAMPLE 17 and 0.5 ml of triethylamine in 25 ml of DCM is cooled to 0-5° C., 0.085 ml of acetyl chloride is added and the mixture is stirred for 3 hours, the temperature being allowed to rise to RT. It is concentrated under vacuum, the residue is taken up with water and extracted with AcOEt, 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 using DCM and then a DCM/MeOH mixture (98/2; 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.=105-107° C.

출처