참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Sodium Iodide | HCID 5238 | — |
| 반응물 | Dimethylformamide | HCID 6228 | — |
| 반응물 | Bromochloromethane | HCID 6333 | — |
| 반응물 | Sodium hydride | HCID 24758 | — |
| 반응물 | Ammonium Chloride | HCID 25517 | — |
| 반응물 | 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 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 생성물 | 6-bromo-8-ethoxy-4H-benzo[1,3]dioxine | HCID 67096800 | — |
반응 단계
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).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US07928228B2 |
|---|
| 출처 데이터셋 | uspto-grants-2011_04 |
|---|
| ORD ID | ord-035d2348da454e09b4cd0f7fbaefe427 |
|---|
| 출처 메모 | uspto-grants-2011_04 |
|---|
