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2-Aminothiophenol → 2-(4-Fluorophenyl)-2H-1,4-benzothiazin-3(4H)-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2-Aminothiophenol | HCID 8713 | — |
| 反応物 | Sodium Acetate | HCID 517045 | — |
| 反応物 | Methyl 2-bromo-2-(4-fluorophenyl)acetate | HCID 12717580 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 2-(4-Fluorophenyl)-2H-1,4-benzothiazin-3(4H)-one | HCID 13690761 | 87.6% |
反応手順
To a suspension of 2-aminothiophenol (12.6 g) and sodium acetate (23.6 g) in ethanol (150 ml) is added methyl α-bromo-4-fluorophenylacetate (23.6 g), and the mixture is stirred at room temperature overnight. After the solvent is distilled off, water is added to the residue. The resulting precipitate is separated by filtration, washed, dried, and then recrystallized from tetrahydrofuran-n-hexane to give 2-(4-fluorophenyl)-3-oxo-3,4-dihydro-2H-1,4-benzothiazine (21.7 g) as crystals. M.p. 216°-219° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05246929 |
| 出典データセット | uspto-grants-1993_09 |
| ORD ID | ord-c9f7e092e3be4773aba7a95c56f0342d |
| 出典メモ | uspto-grants-1993_09 |