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-5-(trifluoromethyl)phenyl]methanol | HCID 29919767 | — |
| 溶媒 | Citric Acid | HCID 311 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 1-(Methanesulfonyloxymethyl)-3-bromo-5-(trifluoromethyl)benzene | HCID 18942164 | 65.6% |
反応手順
Methanesulfonyl chloride (342 mg) was added dropwise to a stirred solution of 3-bromo-5-(trifluoromethyl)benzyl alcohol (560 mg) and triethylamine (417 μl) in dry dichloromethane (20 ml) at -78° C. under a dry nitrogen atmosphere. The reaction was maintained at -78° C. for 30 minutes and then allowed to warm to room temperature over 2 hours. After this period the reaction mixture was diluted with 5% aqueous citric acid and the organic layers were separated, dried over MgSO4, filtered and the solvent removed under reduced pressure to give 1-(methanesulfonyloxymethyl)-3-bromo-5-(trifluoromethyl)benzene as a yellow oil (480 mg) 1H NMR (360 MHz,CDCl3) δ 3.06 (3H,s),5.24 (2H, s), 7.59 (1H, s), 7.75 (1H, s), 7.94 (1H, s).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05830892 |
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| 出典データセット | uspto-grants-1998_11 |
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| ORD ID | ord-a70933ee95ad45b4ab929a9400ac9fed |
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| 出典メモ | uspto-grants-1998_11 |
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