Sodium Hydroxide → 6-[(4,5-Dimethoxy-2-pyridyl)methylthio]-5H-[1,3]-dioxolo[4,5-f]benzimidazole
反応式
[O:1]1[C:13]2[C:4](=[CH:5][C:6]3[NH:10][C:9]([SH:11])=[N:8][C:7]=3[CH:12]=2)[O:3][CH2:2]1.[Cl-].Cl[CH2:16][C:17]1[CH:22]=[C:21]([O:23][CH3:24])[C:20]([O:25][CH3:26])=[CH:19][NH+:18]=1.[OH-].[Na+]>C(O)C.O>[CH3:24][O:23][C:21]1[C:20]([O:25][CH3:26])=[CH:19][N:18]=[C:17]([CH2:16][S:11][C:9]2[NH:10][C:6]3[CH:5]=[C:4]4[O:3][CH2:2][O:1][C:13]4=[CH:12][C:7]=3[N:8]=2)[CH:22]=1参加物
実験手順
A brownish solid is obtained by the procedure described in Example 13 by reaction of 0.85 g of 5H-[1,3]-dioxolo[4,5-f]-benzimidazole-6-thiol with 0.98 g of 2-chloromethyl-4,5-dimethoxypyridinium chloride in 10 ml of ethanol and 10 ml of water, with the addition of 8.5 ml of 1N sodium hydroxide solution, after a reaction time of 20 hours and after concentration, by removing the solvent in vacuo, to a volume of 10 ml. The crude product is dissolved in 30 ml of methylene chloride, the solution is clarified with fuller's earth (for example, Tonsil®), and concentrated. The residue is crystallized by addition of diisopropyl ether and the now pale yellow solid is boiled up in 5 ml of methanol. 0.90 g (60% of theory) of the title compound is obtained as a colorless solid of m.p. 198°-200° C.
後処理
- customA brownish solid is obtained by the procedure
- concentrationafter a reaction time of 20 hours and after concentration
- customby removing the solvent in vacuo
- dissolutionThe crude product is dissolved in 30 ml of methylene chloride
- concentrationconcentrated
- customThe residue is crystallized by addition of diisopropyl ether
出典と根拠
- ORDレコード
- ord-7c401b73e5a3495099bd1247c695ccae
- 出典データセット
- uspto-grants-1988_07
- 特許番号
- US04758579
反応ノート
読み込み中…