تفاعل #1937

معادلة التفاعل

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

المذيبات

DCM

methylene chloride

ظروف التفاعل

المعالجة

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

الإجراء التجريبي

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.).

المصدر