Reaktion #5815

Reaktionsgleichung

sodium chloride

sodium hydride

amorphous compound

N-{1-[(3,4-Dibenzyloxyphenyl)Methyl]-2-(4-Phenylpiperazinyl)Ethyl}-5-Isoquinoline Sulfonamide

methyl iodide

→

title compound

N-{1-[(3,4-Dibenzyloxyphenyl)Methyl]-2-(4-Phenylpiperazinyl)Ethyl}-N-Methyl-5-Isoquinoline Sulfonamide

Lösungsmittel

dimethylformamide

Reaktionsbedingungen

Aufarbeitung

1. 1
   Extraktionthe mixture was extracted with 50 ml of ethyl acetate
2. 2
   WaschenThe extract was washed with saturated sodium chloride aqueous solution
3. 3
   Trocknendried over magnesium sulfate
4. 4
   Einengenconcentrated under a reduced pressure
5. 5
   Sonstigeto obtain a residue, which
6. 6
   Wascheneluted with hexane/ethyl acetate (1:1)

Vorschrift

470 mg of the amorphous compound obtained in Example 5 was dissolved in 8 ml of dimethylformamide, and to the solution were sequentially added 30 mg of 60% sodium hydride and 0.1 ml of methyl iodide with ice cooling, and after stirring for two hours with ice cooling was added saturated sodium chloride, and the mixture was extracted with 50 ml of ethyl acetate. The extract was washed with saturated sodium chloride aqueous solution, dried over magnesium sulfate and concentrated under a reduced pressure to obtain a residue, which was then applied to a silica gel column and eluted with hexane/ethyl acetate (1:1) to obtain 413 mg of the title compound in a colorless amorphous form.

Quelle