化工社化工社 化学情報印刷レポート · 研究参考用
Carbon tetrabromide → 1-(Bromomethyl)-2-fluoro-3-methoxybenzene
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Carbon tetrabromide | HCID 11205 | — |
| 反応物 | Triphenylphosphine | HCID 11776 | — |
| 反応物 | 2-Fluoro-3-methoxybenzyl alcohol | HCID 593589 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 1-(Bromomethyl)-2-fluoro-3-methoxybenzene | HCID 26986100 | — |
反応手順
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.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08106063B2 |
| 出典データセット | uspto-grants-2012_01 |
| ORD ID | ord-2e7cac7b36ec4a1a842112a8a8cfd0e4 |
| 出典メモ | uspto-grants-2012_01 |