化工社化工社 化学情報印刷レポート · 研究参考用
Ammonia → 5-Methoxy-2-(6-methoxybenzothiazol-2-yl)phenylamine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ammonia | HCID 222 | — |
| 反応物 | Stannous chloride dihydrate | HCID 61436 | — |
| 反応物 | 2-Chloro-6-methoxybenzothiazole | HCID 273132 | — |
| 反応物 | 6-Methoxy-2-(4-methoxy-2-nitrophenyl)benzothiazole | HCID 23087377 | — |
| 反応物 | Tributyl(4-methoxy-2-nitrophenyl)tin | HCID 23087474 | — |
| 溶媒 | Hydrochloric Acid | HCID 313 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 5-Methoxy-2-(6-methoxybenzothiazol-2-yl)phenylamine | HCID 23087522 | 75.5% |
反応手順
Synthesized from 2-chloro-6-methoxybenzothiazole and tributyl(4-methoxy-2-nitrophenyl)tin according to an analogous synthetic method to Preparation Example 77, to a suspension of the resulting 6-methoxy-2-(4-methoxy-2-nitrophenyl)benzothiazole (695 mg) in ethanol (10 ml) and concentrated hydrochloric acid (2 ml) was added tin(II) chloride dihydrate (1.3 g), and the solution was stirred for 7 hours at room temperature. The solution was neutralized with ammonia solution on an ice bath, then filtered through celite pad, extracted with ethyl acetate, then sequentially washed with water and brine, the solvent was evaporated in vacuo, the resulting solid was washed with a hexane-diethyl ether system to provide the title compound (475 mg).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07612114B2 |
| 出典データセット | uspto-grants-2009_11 |
| ORD ID | ord-f85a7524f0cc45b089eaff2ca5e047b0 |
| 出典メモ | uspto-grants-2009_11 |