Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
1-Bromo-2,4-dimethoxybenzene → HCID 17968171, 화합물
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 1-Bromo-2,4-dimethoxybenzene | HCID 87266 | — |
| 반응물 | 4-Bromopyridinium chloride | HCID 88100 | — |
| 반응물 | Magnesium | HCID 5462224 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | HCID 17968171 | HCID 17968171 | — |
반응 단계
The Grignard reagent, prepared from magnesium (5 g) and 1-Bromo-2,4-dimethoxybenzene (38 g) in THF (300 ml), is added at room temperature to 4-Bromo-pyridine hydrochloride salt in THF (10 ml). The mixture is heated under reflux for 2 hours and then evaporated to dryness. The residue is taken up in ethyl acetate and extracted with 1N hydrochloric acid. The aqueous phase is neutralised with 4M sodium hydroxide solution and extracted with ethyl acetate. The organic phase is dried with magnesium sulfate, evaporated and the residue is purified by column chromatography on silica gel using n-hexane:AcOEt=1:1 (v/v). MS-APCI+ (M+H)+=216
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07452886B2 |
| 출처 데이터셋 | uspto-grants-2008_11 |
| ORD ID | ord-5fa6046640ef4ac79636829ba2fcab2e |
| 출처 메모 | uspto-grants-2008_11 |