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Salicylamide → 2,2-dimethyl-3,4-dihydro-2H-1,3-benzoxazin-4-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Salicylamide | HCID 5147 | — |
| 反応物 | p-Toluenesulfonic acid | HCID 6101 | — |
| 溶媒 | 2,2-Dimethoxypropane | HCID 6495 | — |
| 生成物 | 2,2-dimethyl-3,4-dihydro-2H-1,3-benzoxazin-4-one | HCID 717428 | — |
反応手順
6.86 g (50 mmol) of salicylamide was suspended in 100 ml of acetone dimethylacetal. After the addition of 2.85 g (15 mmol) of p-toluenesulfonic acid, the mixture was heated to reflux for two hours. The resulting reaction mixture was evaporated under reduced pressure. After the addition of ethyl acetate, the solvent was washed twice with a saturated aqueous solution of sodium hydrogen carbonate and once with brine. The ethyl acetate layer was dried over anhydrous sodium sulfate and the solvent was removed by evaporation under reduced pressure, to obtain 8.94 g (quantitative) of the title compound as light yellow needle-like crystals.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05710152 |
| 出典データセット | uspto-grants-1998_01 |
| ORD ID | ord-c2af07350a1146e78187960312e477d6 |
| 出典メモ | uspto-grants-1998_01 |