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p-Toluenesulfonic acid monohydrate → 2-(4-Fluoro-3-nitrophenyl)benzoxazole
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | p-Toluenesulfonic acid monohydrate | HCID 521998 | — |
| 反応物 | 4-fluoro-N-(2-hydroxyphenyl)-3-nitrobenzanilide | HCID 67497934 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 2-(4-Fluoro-3-nitrophenyl)benzoxazole | HCID 21990970 | 70% |
反応手順
To a suspension of 4-fluoro-N-(2-hydroxyphenyl)-3-nitrobenzanilide (see Working Example 15-1) (2.00 g, 7.24 mmol) in toluene (50 mL) was added p-toluenesulfonic acid monohydrate (2.07 g, 10.9 mmol), and this was stirred and heated to reflux for 4 hours. After the reaction was complete, this was cooled to room temperature, and after the solvent was distilled off, saturated aqueous sodium hydrogen carbonate solution was added and this was stirred for 10 minutes at room temperature. The precipitated crystals were filtered off, and after washing with toluene the crystals were dried to yield the title compound (1.30 g, 70% yield) as yellow crystals.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08829035B2 |
| 出典データセット | uspto-grants-2014_09 |
| ORD ID | ord-503ce20e388a4567b250d68b7b8a3fa5 |
| 出典メモ | uspto-grants-2014_09 |