Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Carbon tetrabromide → 1-(Bromomethyl)-2-fluoro-3-methoxybenzene
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Carbon tetrabromide | HCID 11205 | — |
| 반응물 | Triphenylphosphine | HCID 11776 | — |
| 반응물 | 2-Fluoro-3-methoxybenzyl alcohol | HCID 593589 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 1-(Bromomethyl)-2-fluoro-3-methoxybenzene | HCID 26986100 | — |
반응 단계
Triphenylphosphine (11.1 g) was added to a solution of the subtitle product of step ii) (5.0 g) in DCM (200 ml) followed by the portionwise addition of carbon tetrabromide (14.0 g). The reaction was stirred for 4 h before the addition of further triphenylphosphine (2.0 g) and carbon tetrabromide (2.0 g) and stirring maintained for 1 h. The mixture was concentrated to 30 ml volume and diluted in Et2O (300 ml). The solid precipitate was filtered and washed with Et2O (3×) and the filtrate concentrated in vacuo. The residue was purified by column chromatography (10% Et2O/iso-hexane) to afford the subtitle compound as a clear oil. Yield: 5.2 g.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08106063B2 |
| 출처 데이터셋 | uspto-grants-2012_01 |
| ORD ID | ord-2e7cac7b36ec4a1a842112a8a8cfd0e4 |
| 출처 메모 | uspto-grants-2012_01 |