反応 #1939

反応方程式

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

溶媒

DCM

triethylamine

DCM

反応条件

後処理

1. 1
   濃縮The resulting mixture is concentrated under vacuum
2. 2
   洗浄washed with water, with 1N NaOH solution and with saturated NaCl solution
3. 3
   乾燥dried over MgSO4
4. 4
   濃縮concentrated under vacuum
5. 5
   その他The residue is chromatographed on silica gel H
6. 6
   その他The product obtained
7. 7
   濃縮concentrated under vacuum

実験手順

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.

出典