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Methyl iodide → 6-Bromo-4-methyl-1,4-benzoxazin-3-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 | 6-Bromo-2H-1,4-benzoxazin-3(4H)-one | HCID 16218142 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 6-Bromo-4-methyl-1,4-benzoxazin-3-one | HCID 53217383 | — |
反応手順
To sodium hydride (63 mg) in DMF (3 mL) under an atmosphere of nitrogen was added 6-bromo-2H-benzo[b][1,4]oxazin-3(4H)-one (0.3 g) and the mixture was stirred at room temperature for 1 h. Methyl iodide (0.123 mL) was added and the mixture was stirred overnight at room temperature. The mixture was poured onto ice/water and extracted into ethyl acetate (×2). The ethyl acetate was washed with water (×3), dried and the solvent was evaporated. The resulting material was purified by chromatography on silica eluting with 10% ethyl acetate/isohexane to afford the sub-titled compound (299 mg).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08193239B2 |
| 出典データセット | uspto-grants-2012_06 |
| ORD ID | ord-15e1c4e7f27d4b5d82625a4267c0c832 |
| 出典メモ | uspto-grants-2012_06 |