関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | 4-Chlorophenol | HCID 4684 | — |
| 反応物 | Chloromethylphthalamide | HCID 21973291 | — |
| 触媒 | Zincchloride | HCID 3007855 | — |
| 生成物 | 2-[5-Chloro-2-hydroxy benzyl]isoindole-1,3-dione | HCID 21973298 | — |
反応手順
To 4-chlorophenol (2.0 g, 15.5 mmol) and chloromethylphthalamide (2.62 g, 13.4 mmol) was added zinc chloride (3 mL, 0.5 M in tetrahydrofuran, 1.5 mmol). The reaction was stirred at 90° C. for 48 hours. After cooling the reaction was diluted with methanol (15 mL) and brought to reflux. After 30 minutes the hot suspension was filtered through a medium glass frit and concentrated to an off-white solid. Methanol (50 mL) was again added and the reaction brought to reflux. After 3 hours the hot suspension was filtered through a medium glass frit and concentrated to an off-white solid. The crude product was purified via chromatography on silica gel to give the title compound (3.86 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07098212B2 |
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| 出典データセット | uspto-grants-2006_08 |
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| ORD ID | ord-e670c84d8b25493984d67a7d7e5b877b |
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| 出典メモ | uspto-grants-2006_08 |
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