反応 #78350

反応方程式

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

溶媒

DCM

DCM

反応条件

後処理

1. 1
   その他to rise to RT
2. 2
   濃縮It is concentrated under vacuum
3. 3
   抽出extracted with AcOEt
4. 4
   洗浄the organic phase is washed with water
5. 5
   乾燥dried over Na2SO4
6. 6
   その他the solvent is evaporated off under vacuum
7. 7
   その他The residue is chromatographed on silica
8. 8
   その他The product obtained
9. 9
   その他the precipitate formed
10. 10
    ろ過is filtered off

実験手順

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.

出典