関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Allyl chloride | HCID 7850 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 3-Allyl-5,5-dimethylhydantoin | HCID 597696 | — |
| 反応物 | HCID 178418361 | HCID 178418361 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 1,3-Diallyl-5,5-dimethylhydantoin | HCID 920029 | — |
反応手順
To a slurry of 4.8 grams (0.1 mole) of a 50% sodium hydride mineral oil dispersion in 35 ml. of DMF was added portionwise with stirring 17.6 grams (0.105 mole) of 3-allyl-5,5-dimethylhydantoin. Hydrogen was evolved in this exothermic reaction. The reaction mixture was heated and stirred at 55°-60° C. for 1 hour till the gas evolution ceased and a clear solution resulted. To the solution was added dropwise with stirring over a 10-minute period keeping the temperature below 80° C. 9.3 grams (0.12 mole) of allyl chloride. The reaction mixture was then heated at 55°-60° C. for 1.5 hours. Following cooling to room temperature, the reaction mixture was poured into 100 ml of water. An oily product was formed which was extracted using benzene and purified by vacuum distillation. The above named product was obtained in a yield of 14.15 grams (68%) boiling at 89°-92° C./0.1 mm. (Compound 3)
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04167465 |
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| 出典データセット | uspto-grants-1979_09 |
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| ORD ID | ord-4bf0f6d9855a4f14a9d4d0f5c390f321 |
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| 出典メモ | uspto-grants-1979_09 |
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