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1,2-Dibromoethane → 6-(2-Bromoethoxy)-2,2-dimethyl-2,3-dihydro-4H-1,3-benzoxazin-4-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1,2-Dibromoethane | HCID 7839 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 6-hydroxy-2,2-dimethyl-3,4-dihydro-2H-1,3-benzoxazin-4-one | HCID 13754331 | — |
| 生成物 | 6-(2-Bromoethoxy)-2,2-dimethyl-2,3-dihydro-4H-1,3-benzoxazin-4-one | HCID 13754413 | — |
反応手順
A mixture of 48.2 g of 2,3-dihydro-2,2-dimethyl-6-hydroxy-4H-1,3-benzoxazin-4-one, 70 g of potassium carbonate and 250 ml of 1,2-dibromoethane is refluxed for 4 hours whilst stirring. The semi-liquid reaction mixture is extracted 3 to 4 times whilst hot with 1 liter of methanol each time; the combined methanol extracts are concentrated by evaporation and the residue is recrystallised from methanol. 6-(2-Bromoethoxy)-2,3-dihydro-2,2-dimethyl-4H-1,3-benzoxazin-4-one having a melting point of 190°-195° is obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04727067 |
| 出典データセット | uspto-grants-1988_02 |
| ORD ID | ord-d820998eb2b146de9eeca6c829a21010 |
| 出典メモ | uspto-grants-1988_02 |