反応式
Cl.Cl[C:3]1[N:7]([CH3:8])[CH:6]=[N:5][C:4]=1[S:9]([NH:12][CH2:13][CH2:14][CH2:15][N:16]1[CH2:21][CH2:20][O:19][CH2:18][CH2:17]1)(=[O:11])=[O:10]>[Pd].O>[O:19]1[CH2:18][CH2:17][N:16]([CH2:15][CH2:14][CH2:13][NH:12][S:9]([C:4]2[N:5]=[CH:6][N:7]([CH3:8])[CH:3]=2)(=[O:11])=[O:10])[CH2:21][CH2:20]1参加物
4
実験手順
16.7 g (46.5 mmol) of 5-chloro-N-(3-morpholino-1-propyl)-1-methyl-4-imidazolesulfonamide hydrochloride from Example 32 are hydrogenated at 25° C. and 3.45 bar in the presence of 3 g of Pd/C catalyst in 250 ml of water. The residue remaining after filtration and evaporation in vacuo is converted into the free base using saturated potassium carbonate solution, extracted with dichloromethane and recrystallized from dioxane/diisopropyl ether in order to give the crystalline title compound, identical with that as in Example 7.
後処理
- customare hydrogenated at 25° C.
- filtrationafter filtration and evaporation in vacuo
- extractionextracted with dichloromethane
- customrecrystallized from dioxane/diisopropyl ether in order
出典と根拠
- ORDレコード
- ord-2dbbd33826244a74a46908a270ad0a05
- 出典データセット
- uspto-grants-1994_10
- 特許番号
- US05356922
関連ノート
読み込み中…