関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | Methyl 3-amino-4-hydroxybenzoate | HCID 10815 | — |
| 反応物 | 2-Bromo-2-methylpropionyl bromide | HCID 88685 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | Methyl 2,2-dimethyl-3-oxo-3,4-dihydro-2h-1,4-benzoxazine-6-carboxylate | HCID 10513902 | 80.3% |
反応手順
To solution of 2-amino-4-methoxycarbonylphenol [Acta Chimica Academiae Scientiarum Hungaricae, 99 (1), 49-50 (1979)] (4.78 g) in a mixed solvent of ethyl acetate (50 ml) and water (50 ml) were added sodium hydrogen carbonate (3.6 g) and 2-bromoisobutyryl bromide (6.90 g) and the mixture was stirred at room temperature for 10 minutes. The organic layer was separated and the solvent was distilled off under reduced pressure. The resulting residue was dissolved in dimethylformamide (70 ml), to the solution was added potassium carbonate (4.35 g) and the mixture was stirred at room temperature for a day. The reaction solution was poured into water to give precipitates, which were taken by filtration and dried to give 2,2-dimethyl-6-methoxycarbonyl-3-oxo-3,4-dihydro-2H-1,4-benzoxazine (5.4 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US05597820 |
|---|
| 出典データセット | uspto-grants-1997_01 |
|---|
| ORD ID | ord-c62b92fd63cc49bab014604fcad2e63b |
|---|
| 出典メモ | uspto-grants-1997_01 |
|---|