反应 #78350

反应方程式

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

溶剂

DCM

DCM

反应条件

后处理

1. 1
   其他to rise to RT
2. 2
   浓缩It is concentrated under vacuum
3. 3
   萃取extracted with AcOEt
4. 4
   洗涤the organic phase is washed with water
5. 5
   干燥dried over Na2SO4
6. 6
   其他the solvent is evaporated off under vacuum
7. 7
   其他The residue is chromatographed on silica
8. 8
   其他The product obtained
9. 9
   其他the precipitate formed
10. 10
    过滤is filtered off

实验过程

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.

来源