Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Water → 5-Bromo-8-methoxy-2,3-dihydrobenzo[B][1,4]dioxine
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | 1,2-Dibromoethane | HCID 7839 | — |
| 반응물 | Potassium Fluoride | HCID 522689 | — |
| 반응물 | 3-Bromo-6-methoxybenzene-1,2-diol | HCID 3705874 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | 5-Bromo-8-methoxy-2,3-dihydrobenzo[B][1,4]dioxine | HCID 2825015 | — |
반응 단계
3-bromo-6-methoxycatechol (16 g) was dissolved in DMF (50 ml), mixed with 1,2-dibromoethane (15 ml) and potassium fluoride (21 g), stirred for 6 hours while heating at 110EC. The resultant was allowed to stand for cooling, mixed with water, and extracted with ether. The organic layer was washed withan aqueous sodium hydroxide solution, water, and a saturated aqueous sodium chloride solution in that order, dried over manganese sulfate anhydride, and then, evaporated under reduced pressure for removing the solvent. The residue was purified by silica gel column chromatography (hexane/ethyl acetate=4/1) to give Compound IIbo-a (5.9 g, 34%) as a white solid.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US06514996B2 |
| 출처 데이터셋 | uspto-grants-2003_02 |
| ORD ID | ord-6e4b48aa994847d780c89c5b74975537 |
| 출처 메모 | uspto-grants-2003_02 |