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Triethylamine → 3-Bromo-4-fluorobenzyl methanesulfonate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Methanesulfonyl chloride | HCID 31297 | — |
| 反応物 | 3-Bromo-4-fluorobenzyl Alcohol | HCID 2773351 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 3-Bromo-4-fluorobenzyl methanesulfonate | HCID 59854813 | 82.1% |
反応手順
To a solution of (3-bromo-4-fluorophenyl)methanol (53 g, 0.258 mol) in DCM (500 mL) at 0° C. was added Et3N (108 mL, 775 mmol, 3 eq) and methanesulfonyl chloride (24 mL, 310 mmol, 1.2 eq) successively. After stirring 30 min, the reaction mixture was partitioned in DCM and water. The organic layer was dried over MgSO4 and evaporated in vacuo to give 3-bromo-4-fluorobenzyl methanesulfonate (60 g), which used to the next step without further purification. 1H NMR (400 MHz, CDCl3) δ 7.65-7.62 (m, 1H), 7.37-7.33 (m, 1H), 7.16 (t, J=4.4 Hz, 1H), 5.17 (s, 2H), 2.99 (s, 3H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08846739B2 |
| 出典データセット | uspto-grants-2014_09 |
| ORD ID | ord-ec7499c6f61a4e40a8ae183568bf4d73 |
| 出典メモ | uspto-grants-2014_09 |