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Triethylamine → 2-(Chloromethyl)-5-(4-(trifluoromethyl)phenyl)thiophene
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 | 2-Thiophenemethanol, 5-[4-(trifluoromethyl)phenyl]- | HCID 21986352 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 2-(Chloromethyl)-5-(4-(trifluoromethyl)phenyl)thiophene | HCID 57594979 | — |
反応手順
To a mixture of [5-(4-Trifluoromethyl-phenyl)-thiophen-2-yl]-methanol (1.52 g, 5.89 mmole) and triethyl amine (1.64 mL, 11.78 mmole) in DCM (100 mL) at 0° C., is injected methanesulfonyl chloride (0.91 mL, 11.78 mmole) dropwise. The reaction is kept at 0° C. for an hour and warmed up to room temperature for an hour. The reaction mixture is concentrated on rota vapor, and the resulting residue is purified on a silica gel column, eluting with 0-15% ethyl acetate in hexane and concentrated to provide the titled compound as off-white solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07504433B2 |
| 出典データセット | uspto-grants-2009_03 |
| ORD ID | ord-98d68cde2bec498d802059a64c64ffde |
| 出典メモ | uspto-grants-2009_03 |