반응 #1937

반응 방정식

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

용매

DCM

methylene chloride

반응 조건

후처리

1. 1
   세척the reaction mixture is washed with water
2. 2
   건조with 10% Na2CO3 solution and the organic phase is dried over MgSO4
3. 3
   농축concentrated under vacuum
4. 4
   기타The residue is chromatographed on silica gel H
5. 5
   기타The product obtained
6. 6
   농축concentrated under vacuum

실험 절차

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.).

출처