化工社化工社 化学情報印刷レポート · 研究参考用
Acetyl chloride → 1-(6-nitro-2H-benzo[b][1,4]oxazin-4(3H)-yl)ethanone
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Acetyl chloride | HCID 6367 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | 6-nitro-3,4-dihydro-2H-1,4-benzoxazine | HCID 7062225 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 1-(6-nitro-2H-benzo[b][1,4]oxazin-4(3H)-yl)ethanone | HCID 57864714 | 90% |
反応手順
Under vigorous stirring at room temperature, acetyl chloride (1.02 g, 13 mmol) was added dropwise to a mixture of 6-nitro-3,4-dihydro-2H-benzo[1,4]oxazine (1.8 g, 10 mmol) and NaHCO3 (7.14 g, 85 mmol) in CH2Cl2 (50 mL). After addition, the reaction was stirred for 1 h at this temperature. The mixture was filtered and the filtrate was concentrated under vacuum. The residue was treated with Et2O:hexane (1:2, 50 mL) under stirring for 30 min and then filtered to give 4-acetyl-6-nitro-3,4-dihydro-2H-benzo[1,4]oxazine as a pale yellow solid (2 g, 90%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08829204B2 |
| 出典データセット | uspto-grants-2014_09 |
| ORD ID | ord-7ccda5df6a2047b99cc019ca9cb59536 |
| 出典メモ | uspto-grants-2014_09 |