تفاعل #1938

معادلة التفاعل

hydrochloric ether

triethylamine

compound

4-Acetamido-4-phenyl-1-[2-[1-(3,4-dichlorophenyl)-2-(N-methylamino)ethoxy]ethyl]piperidine dihydrochloride

benzyl chloroformate

→

hydrochloride

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

المذيبات

DCM

DCM

ظروف التفاعل

المعالجة

1. 1
   غسيلThe reaction mixture is washed twice with water
2. 2
   تجفيفdried 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

0.41 ml of triethylamine is added to a solution of 0.5 g of the compound obtained in EXAMPLE 11, step B), in 10 ml of DCM, the mixture is then cooled to 0° C. and 0.14 ml of benzyl chloroformate is added dropwise. The reaction mixture is washed twice with water, dried over MgSO4 and concentrated under vacuum. The residue is chromatographed on silica gel H using DCM and then a DCM/MeOH mixture (94/6; 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 0.39 g of the expected hydrochloride after crystallization from iso ether. M.p.=135° C.

المصدر