反応 #1937

反応方程式

hydrochloric ether

triethylamine

propionyl chloride

compound

4-Hydroxy-4-phenyl-1-[2-[1-(3,4-dichlorophenyl)-2-(N-methyl-N-benzyloxycarbonylamino)ethoxy]ethyl]piperidine hydrochloride

→

hydrochloride

4-Phenyl-4-propionyloxy-1-[2-[1-(3,4-dichlorophenyl)-2-(N-methyl-N-benzyloxycarbonylamino)ethoxy]ethyl]piperidine hydrochloride hemihydrate

溶媒

DCM

methylene chloride

反応条件

後処理

1. 1
   洗浄the reaction mixture is washed with water
2. 2
   乾燥with 10% Na2CO3 solution and the organic phase is dried over MgSO4
3. 3
   濃縮concentrated under vacuum
4. 4
   その他The residue is chromatographed on silica gel H
5. 5
   その他The product obtained
6. 6
   濃縮concentrated under vacuum

実験手順

670 mg of the compound obtained in EXAMPLE 9 are dissolved in 10 ml of methylene chloride, and 0.2 ml of triethylamine and 0.2 ml of propionyl chloride are then added, with stirring. After 15 minutes, the reaction mixture is washed with water and then with 10% Na2CO3 solution and the organic phase is dried over MgSO4 and concentrated under vacuum. The residue is chromatographed on silica gel H using DCM and then a DCM/MeOH mixture (97/3; v/v) as the eluent. The product obtained is taken up with DCM, acidified to pH 1 by the addition of hydrochloric ether and concentrated under vacuum to give 0.52 g of the expected hydrochloride after crystallization from pentane. M.p.=115° C. (dec.).

出典