反応 #5815

反応方程式

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

溶媒

dimethylformamide

反応条件

後処理

1. 1
   抽出the mixture was extracted with 50 ml of ethyl acetate
2. 2
   洗浄The extract was washed with saturated sodium chloride aqueous solution
3. 3
   乾燥dried over magnesium sulfate
4. 4
   濃縮concentrated under a reduced pressure
5. 5
   その他to obtain a residue, which
6. 6
   洗浄eluted with hexane/ethyl acetate (1:1)

実験手順

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.

出典