化工社化工社 化学情報印刷レポート · 研究参考用
Dimethylformamide → 2,7-dimethoxy-3H-phenothiazin-3-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | 2-Methoxy-1,4-benzoquinone | HCID 76146 | — |
| 反応物 | 2-Amino-5-methoxybenzene-1-thiol | HCID 235509 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 2,7-dimethoxy-3H-phenothiazin-3-one | HCID 12199923 | — |
反応手順
To a suspension of 2-methoxy-p-benzoquinone (1.15 kg) (Step 1) in methanol (8 l) was added portionwise a suspension of 2-amino-5-methoxythiophenol (from Step 2) in methanol (6 l). The reacting mixture was stirred for 15 minutes, filtered and washed with methanol (8 l). The product isolated was swished with DMF (16 l) for 2 hours, filtered and air-dried. The crude material was dissolved in hot DMF (16 l) (130°-140° C.), filtered on Celite and the filtrate cooled to room temperature. The resulting crystals were filtered, washed with methanol (8 l) and air-dried to afford the title compound (70.3 g), m.p. 237°-238° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04845083 |
| 出典データセット | uspto-grants-1989_07 |
| ORD ID | ord-1e5ec47aeb7d4438b19702d3e772f9dc |
| 出典メモ | uspto-grants-1989_07 |