Реакция #1939

Уравнение реакции

hydrochloric ether

BOP

compound

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

phenylacetic acid

→

hydrochloride

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

Растворители

DCM

triethylamine

DCM

Условия реакции

Обработка

1. 1
   КонцентрированиеThe resulting mixture is concentrated under vacuum
2. 2
   Промывкаwashed with water, with 1N NaOH solution and with saturated NaCl solution
3. 3
   Сушкаdried over MgSO4
4. 4
   Концентрированиеconcentrated under vacuum
5. 5
   ДругоеThe residue is chromatographed on silica gel H
6. 6
   ДругоеThe product obtained
7. 7
   Концентрированиеconcentrated under vacuum

Методика

0.46 ml of triethylamine and then 0.5 g of BOP are added to a mixture of 0.5 g of the compound obtained in EXAMPLE 11, step B), 0.127 g of phenylacetic acid and 10 ml of DCM. The resulting mixture is concentrated under vacuum and the residue is taken up with AcOEt, washed with water, with 1N NaOH solution and with saturated NaCl solution, 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 0.42 g of the expected hydrochloride after crystallization from iso ether. M.p.=125° C.

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