関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Iodoethane | HCID 6340 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 3,4-Dihydro-2H-1,4-benzoxazine | HCID 585096 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 4-ethyl-3,4-dihydro-2H-benzo[1,4]oxazine | HCID 12948877 | 55.9% |
反応手順
To a stirred solution of 3,4-dihydro-2H-benzo[1,4]oxazine (4.0 g, 29.6 mmol) in DMF (20 ml) was added potassium carbonate (10.22 g, 74.0 mmol). After stirring for five min. Iodo-ethane (3.5 ml, 44.4 mmol) was added and heated to 60° C. for overnight. Reaction mixture was cooled to room temperature, quenched by the addition of water (20 ml), extracted with ethyl acetate (3×25 ml). The organic layer was washed with water (30 ml), brine (30 ml), dried over sodium sulfate, concentrated and purified by silica gel column chromatography to furnish 4-ethyl-3,4-dihydro-2H-benzo[1,4]oxazine (2.7 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08394772B2 |
|---|
| 出典データセット | uspto-grants-2013_03 |
|---|
| ORD ID | ord-c84874e32e654e8f9e1d870cb4535965 |
|---|
| 出典メモ | uspto-grants-2013_03 |
|---|