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Triethylamine → N-{4-[3-(4-pentafluorosulphanyl-benzyl)-thioureidomethyl]-2-fluoro-phenyl}-methane sulphonamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | N-(4-(aminomethyl)-2-fluorophenyl)methanesulfonamide | HCID 21097526 | — |
| 反応物 | 4-(Pentafluorosulphanyl)benzylisothiocyanate | HCID 86630633 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | N-{4-[3-(4-pentafluorosulphanyl-benzyl)-thioureidomethyl]-2-fluoro-phenyl}-methane sulphonamide | HCID 16097202 | — |
反応手順
N-(4-aminomethyl-2-fluoro-phenyl)-methane sulphonamide (237 mg, 1.09 mmol) was dissolved in dimethylformamide (1 ml) and to this was added triethylamine (132 mg, 1.30 mmol) and 4-(pentafluorosulphanyl)benzylisothiocyanate (300 mg, 1.09 mmol) dissolved in dimethylformamide (1 ml). The reaction mixture was stirred over night at room temperature, the solvent removed under vacuum and the residue dissolved in a little methanol. Following column chromatographic cleaning (silica gel, hexane/ethyl acetate 1:5), the product was obtained as a solid (305 mg, 57% of the theoretical amount).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07994167B2 |
| 出典データセット | uspto-grants-2011_08 |
| ORD ID | ord-5f635046761445698db3a187c64b2c9c |
| 出典メモ | uspto-grants-2011_08 |