関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Thionyl Chloride | HCID 24386 | — |
| 反応物 | Hydroxyammonium hydrochloride | HCID 22029257 | — |
| 反応物 | 2-Chloro-4-fluoro-3-formylbenzonitrile | HCID 59370491 | — |
| 溶媒 | N-methyl-2-pyrrolidone | HCID 13387 | — |
| 生成物 | 2-Chloro-4-fluoroisophthalonitrile | HCID 59370516 | 85.7% |
反応手順
To a solution of 2-chloro-4-fluoro-3-formylbenzonitrile (597 mg) in 1-methyl-2-pyrrolidone (10 mL) was added hydroxyammonium hydrochloride (310 mg), and the mixture was stirred at 100° C. for 1 hr. The reaction mixture was ice-cooled at 0° C., and thionyl chloride (0.735 mL) was added dropwise thereto. The mixture was stirred at the same temperature for 30 min, water was added to the mixture and the mixture was extracted with ethyl acetate. The extract was washed with saturated brine, dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The residue was recrystallized from hexane to give the title compound as yellow crystals (yield: 503 mg).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08592452B2 |
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| 出典データセット | uspto-grants-2013_11 |
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| ORD ID | ord-2d959a47e1454b45a70ae576f3d5d1ae |
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| 出典メモ | uspto-grants-2013_11 |
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