化工社化工社 化学情報印刷レポート · 研究参考用
Hydrochloric Acid → 10H-Thieno[2,3-b][1,5]benzodiazepin-4-amine, 2-methyl-, hydrochloride (1:1)
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 5-Methyl-2-((2-nitrophenyl)amino)-3-thiophenecarbonitrile | HCID 395460 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 10H-Thieno[2,3-b][1,5]benzodiazepin-4-amine, 2-methyl-, hydrochloride (1:1) | HCID 135525650 | — |
反応手順
To a stirred slurry of 2-(2-nitroanilino)-5-methyl-thiophene-3-carbonitrile (3 g, 0.011 mol) in ethanol (35 mL) at 50° C. was added, over 10 minutes, a solution of anhydrous stannous chloride (6.95 g, 0.037 mol) in hydrochloric acid (26 mL, 5M). The mixture was stirred under reflux for 1 hour, concentrated under reduced pressure and allowed to crystallize over night at 5° C. The salt was filtered, washed with a small amount of water, dried (4.3 g) m.p. >250° C., and used without further purification in the next stage.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05817655 |
| 出典データセット | uspto-grants-1998_10 |
| ORD ID | ord-30863290fb02423d85731815bd21079d |
| 出典メモ | uspto-grants-1998_10 |