Реакция #1938

Уравнение реакции

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

Растворители

DCM

DCM

Условия реакции

Обработка

1. 1
   ПромывкаThe reaction mixture is washed twice with water
2. 2
   Сушкаdried over MgSO4
3. 3
   Концентрированиеconcentrated under vacuum
4. 4
   ДругоеThe residue is chromatographed on silica gel H
5. 5
   ДругоеThe product obtained
6. 6
   Концентрированиеconcentrated under vacuum

Методика

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.

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