関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Iodide | HCID 5238 | — |
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | Bromochloromethane | HCID 6333 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | Ammonium Chloride | HCID 25517 | — |
| 反応物 | 2-{3-[(4-carbamimidoylphenylamino)-(2-fluoro-4,5-dimethoxyphenyl)methyl]5-oxo-4,5-dihydro-[1,2,4]triazol-1-yl}benzoic Acid Trifluoroacetate | HCID 136337083 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 6-bromo-8-ethoxy-4H-benzo[1,3]dioxine | HCID 67096800 | — |
反応手順
To a solution of this compound in 40 ml of DMF there was added 1g of sodium hydride (60% oily suspension) while cooling on ice, and the mixture was stirred at room temperature for 30 minutes. After then adding 1 ml of bromochloromethane and 0.25 g of sodium iodide to the reaction mixture, it was stirred at 80° C. for 6 hours under a hydrogen atmosphere. Saturated aqueous ammonium chloride was added to the reaction mixture, and extraction was performed with ethyl acetate. The organic layer was dried over anhydrous magnesium sulfate. The desiccating agent was filtered off and the filtrate was concentrated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate-heptane) to give 6-bromo-8-ethoxy-4H-benzo[1,3]dioxine (1.62 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07928228B2 |
|---|
| 出典データセット | uspto-grants-2011_04 |
|---|
| ORD ID | ord-035d2348da454e09b4cd0f7fbaefe427 |
|---|
| 出典メモ | uspto-grants-2011_04 |
|---|
