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Methyl iodide → 5,6-Dichloro-1-methylisatin
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 | 5,6-dichloro-1H-indole-2,3-dione | HCID 11009341 | — |
| 反応物 | HCID 178418361 | HCID 178418361 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 5,6-Dichloro-1-methylisatin | HCID 22274384 | 81% |
反応手順
To a solution of 5,6-dichloroisatin (0,15 g; 0.7 mmol) in anhydrous DMF (5 ml) was added sodium hydride (40 mg, 60% dispersion in mineral oil). When the evolution of hydrogen had ceased iodomethane (0.1 ml) was added and the mixture was stirred for 20 min. at ambient temperature. Water (15 ml) and glacial acetic acid (0.1 ml) were added and the product was filtered off, washed with water and dried to yield 5,6-dichloro-1-methylisatin (0.13 g, 81%). The following compounds were prepared analogously: 4,5-dichloro-1-methylisatin (2b) from 4,5-dichloroisatin, and 6,7-dichloro-1-methylisatin from 6,7-dichloroisatin.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06969729B2 |
| 出典データセット | uspto-grants-2005_11 |
| ORD ID | ord-2dd4f14ba8ea4157b63e9421531775bc |
| 出典メモ | uspto-grants-2005_11 |