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HRID 430472作成日：2026年10月26日
Hydrochloric Acid → 5-[2-Hydroxy-4-(5-fluoro-2-methoxyphenyl)-4-methyl-2-methyl-pentylamino]-phthalide
https://huagongshe.com/reaction/430472
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 5-Acetamido-phthalide | HCID 590968 | — |
| 反応物 | 4-Toluenesulfonic acid-[2-hydroxy-4-(5-fluoro-2-methoxyphenyl)-2-trifluoromethyl-pentyl]-ester | HCID 18350645 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 5-[2-Hydroxy-4-(5-fluoro-2-methoxyphenyl)-4-methyl-2-methyl-pentylamino]-phthalide | HCID 18350657 | — |
反応手順
688 mg of 5-acetamidophthalide in 15 ml of dimethylformamide is mixed under argon at 0° C. with 108 mg of an 80% sodium hydride/oil suspension. After 10 minutes of stirring at this temperature, 556 mg of 4-toluenesulfonic acid-[2-hydroxy-4-(5-fluoro-2-methoxyphenyl)-2-trifluoromethyl-pentyl]-ester is added. After 16 hours of stirring at 60° C., it is added to 1 M hydrochloric acid, neutralized with potassium carbonate and extracted with ethyl acetate. After drying (Na2SO4), the crude product is chromatographed on silica gel. With hexane/ethyl acetate (60:40), the title compound is obtained in a crystalline state, flash point 148-149° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06323199B1 |
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| 出典データセット | uspto-grants-2001_11 |
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| ORD ID | ord-2f3204f144704d4e8ba7a9135a48a5be |
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| 出典メモ | uspto-grants-2001_11 |
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