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Methyl iodide → 6-chloro-7-methylsulfanyl-3-trifluoromethyl-1H-quinoxalin-2-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methyl iodide | HCID 6328 | — |
| 反応物 | 4-Chloro-5-fluoro-1,2-phenylenediamine | HCID 735773 | — |
| 反応物 | Ethyl 3,3,3-trifluoro-2-oxopropanoate | HCID 2737239 | — |
| 反応物 | Sodium hydrogen sulfide hydrate | HCID 53442613 | — |
| 反応物 | HCID 178517239 | HCID 178517239 | — |
| 反応物 | HCID 178517316 | HCID 178517316 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 6-chloro-7-methylsulfanyl-3-trifluoromethyl-1H-quinoxalin-2-one | HCID 22341150 | 38% |
反応手順
A mixture of 6-chloro-7-fluoro-3-trifluoromethyl-quinoxalin-2-ol and 7-chloro-6-fluoro-3-trifluoromethyl-quinoxalin-2-ol (4.1 g, prepared similarly as described above from 4-chloro-5fluoro-1,2-diaminobenzene and ethyl trifluoropyruvate) was dissolved in DMF (140 ml) and sodium hydrogen sulfide monohydrate (3.5 g, 47 mmol) was added. The reaction mixture was stirred at room temperature for 1 hour and then iodomethane (3.5 ml) was added. Stirring was continued for 10 minutes and the reaction mixture was poured on ice/water (500 ml). The separated crystals were filtered, dried and recrystallised from ethanol to afford 1.73 g (38%) of 6-chloro-7-methylsulfanyl-3-trifluoromethyl-1H-quinoxalin-2-one.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06927214B1 |
| 出典データセット | uspto-grants-2005_08 |
| ORD ID | ord-6c0033fd1fff4e99a6ba8ec915762f25 |
| 出典メモ | uspto-grants-2005_08 |