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Lawesson's reagent → 4-amino-N-(3-bromo-4-fluorophenyl)-1,2,5-thiadiazole-3-carbothioamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Lawesson's reagent | HCID 87949 | — |
| 反応物 | 4-amino-N-(3-bromo-4-fluorophenyl)-1,2,5-thiadiazole-3-carboxamide | HCID 58558244 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 4-amino-N-(3-bromo-4-fluorophenyl)-1,2,5-thiadiazole-3-carbothioamide | HCID 58558309 | 55.7% |
反応手順
A solution of 4-amino-N-(3-bromo-4-fluorophenyl)-1,2,5-thiadiazole-3-carboxamide (225 mg, 0.7 mmol) and 2,4-bis(4-methoxyphenyl)-2,4-dithioxo-1,3,2,4-dithiadiphosphetane (570 mg, 1.4 mmol) in toluene (6.8 mL) was stirred at 95° C. for 16 h. The reaction mixture was diluted with ethyl acetate (50 mL) and the insoluble salts were filtered. The filtrate was concentrated to a crude residue which was purified on silica gel to give the desired product (130 mg, 55%). LCMS for C9H7BrFN4S2 (M+H)+: m/z=332.8, 334.9.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08846726B2 |
| 出典データセット | uspto-grants-2014_09 |
| ORD ID | ord-bf4e5550eb00476595e5c06b5f2e6286 |
| 出典メモ | uspto-grants-2014_09 |