반응 #1939

반응 방정식

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

용매

DCM

triethylamine

DCM

반응 조건

후처리

1. 1
   농축The resulting mixture is concentrated under vacuum
2. 2
   세척washed with water, with 1N NaOH solution and with saturated NaCl solution
3. 3
   건조dried over MgSO4
4. 4
   농축concentrated under vacuum
5. 5
   기타The residue is chromatographed on silica gel H
6. 6
   기타The product obtained
7. 7
   농축concentrated under vacuum

실험 절차

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.

출처