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Pyridine → 2,6-Dibromo-4-fluorobenzyl acetate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Pyridine | HCID 1049 | — |
| 反応物 | Acetyl chloride | HCID 6367 | — |
| 反応物 | (2,6-Dibromo-4-fluorophenyl)methanol | HCID 58043943 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 2,6-Dibromo-4-fluorobenzyl acetate | HCID 67016593 | 87% |
反応手順
To a solution of (2,6-dibromo-4-fluorophenyl)methanol (104l) (20 g, 71 mmol) in CH2Cl2 (500 mL) at 0° C. was added pyridine (8.4 g, 107 mmol) and acetyl chloride (8.3 g, 107 mmol). The mixture was stirred at room temperature for 5 h. TLC showed the start material disappeared. The reaction was evaporated in vacuum and the residue was purified by silica-gel column chromatography eluting with petroleum ether/ethyl acetate (from 50:1 to 20:1) to give 104m as a white solid (20g, 87%). MS: [M-Oac]+ 267. 1H NMR (500 MHz, CDCl3) δ 7.36 (d, J=7.5, 2H), 5.38 (s, 2H), 2.10 (s, 3H)
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09115152B2 |
| 出典データセット | uspto-grants-2015_08 |
| ORD ID | ord-ffc4a879204b4765ba6bc3529aa5ae70 |
| 出典メモ | uspto-grants-2015_08 |