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Methyl iodide → 6-Amino-4-methyl-2H-1,4-benzothiazin-3(4H)-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methyl iodide | HCID 6328 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | Ammonium Chloride | HCID 25517 | — |
| 反応物 | 6-amino-3,4-dihydro-2H-1,4-benzothiazin-3-one | HCID 686901 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 6-Amino-4-methyl-2H-1,4-benzothiazin-3(4H)-one | HCID 21988147 | 63.9% |
反応手順
4.5 g 6-Amino-4H-benzo[1,4]thiazin-3-one in 50 ml DMF was treated in portions with 0.695 g 95% sodium hydride at room temperature. After 30 min, 3.548 g methyl iodide were added dropwise at 0° C. and stirring was continued for another 30 min. The mixture was poured into ice and ammonium chloride solution and extracted with CH2Cl2. Chromatography on silica yielded 3.1 g crude product, which was further purified by trituration with diethyl ether.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07091345B2 |
| 出典データセット | uspto-grants-2006_08 |
| ORD ID | ord-ae7541c76b774e8fa0cc87517c966110 |
| 出典メモ | uspto-grants-2006_08 |