関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ibuprofen, (+-)- | HCID 3672 | — |
| 反応物 | Sodium Chloride | HCID 5234 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Ammonium Persulfate | HCID 62648 | — |
| 反応物 | Sodium | HCID 5360545 | — |
| 反応物 | 2-Acetoxy-3-methyl-3-(p-isobutylphenyl)acrylonitrile | HCID 53777324 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Diglyme | HCID 8150 | — |
| 生成物 | Ibuprofen, Sodium Salt | HCID 5338317 | — |
反応手順
A portion of the enol-acetate solution (V) from A above, (55.41 g. representing 49.3 mmole of enol-acetate) was placed in a 250 ml. 1 necked flask and stirred magnetically while 10 ml. of saturated sodium chloride solution and 16.0 g. of 50 percent sodium hydroxide (200 meq.) were added. The mixture was stirred and allowed to cool to 25° C. and the ammonium persulfate [(NH4)2S2O8 ] (12.5 g.; 55 meq.) in 16 ml. of water were added over 10 minutes. After stirring overnight, 10 ml. of diglyme was added and the pH was adjusted from 9 to 13. The mixture was slowly cooled to 0° C. with seeding with crystals of 2-(4'-isobutylphenyl)propionic acid, sodium salt and held at 0° C. for 3 hours to form solid sodium 2-(4'-isobutylphenyl)propionate (VI) as a crystalline precipitate.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US03987094 |
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| 出典データセット | uspto-grants-1976_10 |
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| ORD ID | ord-873fe138cbda45109326e511d61118a2 |
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| 出典メモ | uspto-grants-1976_10 |
|---|