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Hydrogen Bromide → 5-Ethyl-5-(3-bromopropyl)barbituric acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrogen Bromide | HCID 260 | — |
| 反応物 | 2,4,6(1H,3H,5H)-Pyrimidinetrione, 5-ethyl-5-(2-propenyl)- | HCID 48542 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 5-Ethyl-5-(3-bromopropyl)barbituric acid | HCID 19911801 | — |
反応手順
A suspension of 40 g of 5-ethyl-5-allylbarbituric acid and 800 ml of toluene was stirred and irradiated with a GE sunlamp (275 watts, 110-125 volts) for approximately 90 min. Thereafter, gaseous HBr was passed for 45 min. with further irradiation and stirred for another 45 minutes. The reaction flask was then opened to allow the excess HBr to evaporate. The solution was cooled and filtered. The resulting precipitate was washed with toluene, dried, and then dissolved in a minimal amount of hot acetone. Petroleum ether (60°-68° C.) was added until a small amount of precipitate appeared; the flask was left overnight at 23° C. The crystals were filtered, washed with petroleum ether, and air dried. The melting point was 138°-140° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05110914 |
| 出典データセット | uspto-grants-1992_05 |
| ORD ID | ord-88bd73ad002446f4ae22af412c49a706 |
| 出典メモ | uspto-grants-1992_05 |