関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | O-Phenylenediamine | HCID 7243 | — |
| 反応物 | 1,2-Phenylenediamine dihydrochloride | HCID 11990 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 4-Cyanothiazole | HCID 15069 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | Thiabendazole | HCID 5430 | 77.5% |
反応手順
To a 1 liter four-neck flask equipped with a mechanical stirrer, a condenser, pH probe and thermometer were added 54 grams (0.5 mole) of 4-cyanothiazole, 90.5 grams (0.5 mole) of o-phenylenediamine dihydrochloride and 250 ml of deionized water. Sodium hydroxide pellets were added in sufficient proportion to increase the pH of the reaction mixture to a value of 4.0. The mixture was heated to reflux and held at reflux (100°-102° C.) for 4 hours. The reaction was determined to be complete when the peaks corresponding to o-phenylenediamine and 4-cyanothiazole were absent from the gas chromatogram. The reaction mass was allowed to cool to room temperature before adding 0.1N NaOH to adjust the pH to a value within a range of 8-10. The product was filtered, washed three times with 300 ml portions of deionized water, and then dried overnight in a vacuum oven. A total of 78.0 grams of thiabendazole were obtained which corresponds to a 77.5% yield.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05310924 |
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| 出典データセット | uspto-grants-1994_05 |
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| ORD ID | ord-bd02c7687bd94a1ea592eff0ff07e3d4 |
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| 出典メモ | uspto-grants-1994_05 |
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