関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Propylene Oxide | HCID 6378 | — |
| 反応物 | 5-Ethyl-5-methylhydantoin | HCID 82162 | — |
| 触媒 | Hydrochloric Acid | HCID 313 | — |
| 触媒 | Lithium Chloride | HCID 433294 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 1,3-Di-(beta-hydroxy-n-propyl)-5-ethyl-5-methylhydantoin | HCID 23338221 | 99.7% |
反応手順
A mixture of 256.3 g of 5ethyl-5-methylhydantoin (1.805 mols), 675 ml of dimethylformamide and 4.51 g of lithium chloride is stirred at 50° C. 288.0 g of propene oxide (4.96 mols) are slowly added dropwise over the course of 2 hours. Thereafter the temperature is gradually raised to 90° C. over the course of 10 hours. The reaction mixture is brought to pH = 7 with 4 drops of 2 N hydrochloric acid, filtered and concentrated on a rotational evaporator at 90° C. bath temperature, under a waterpumpvacuum. It is then treated at 90° C. under 0.1 mm Hg until the weight remains constant. 465 g of a clear pale yellow product (99.5% of theory) are obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04161594 |
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| 出典データセット | uspto-grants-1979_07 |
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| ORD ID | ord-0ea8014758ba41adb59aef4c49adc2cc |
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| 出典メモ | uspto-grants-1979_07 |
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