関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2-Chloroethyl vinyl ether | HCID 8074 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 5-Ethyl-5-methylhydantoin | HCID 82162 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 3-[2-(Vinyloxy)-ethyl]-5-methyl-5-ethyl-hydantoin | HCID 20285622 | — |
反応手順
A mixture of 71.04 g (0.5 mol) of 5-methyl-5-ethylhydantoin, 55.94 g (0.5 mol+5% excess) of 2-chloroethyl vinyl ether, 36.28 g (0.25 mol+5% excess) of anhydrous potassium carbonate and 150 ml of dimethylformamide is stirred, analogously to Example 1, for 4 hours and 35 minutes at 122°-129° C. After completion of the reaction, the reaction mixture is filtered and the clear filtrate is concentrated on a rotary evaporator at 80° C. under vacuum from a waterpump. The residue is taken up in 200 ml of acetone, 2 g of active charcoal are added and the mixture is kept at the boil for 15 minutes. It is then filtered and the filtrate is concentrated on a rotary evaporator at 60° C. under vacuum from a waterpump. The residue is freed from non-volatile constituents at 60° C. and 0.5 mm Hg and 86.9 g (81.9% of theory) of a yellowish, viscous crude product are obtained. This is purified by distillation in a high vacuum and 80.34 g (75.7% of theory) of the desired product, of boiling point 132° C./0.2 mm Hg, are obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04206309 |
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| 出典データセット | uspto-grants-1980_06 |
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| ORD ID | ord-7a2e746716a5498dbdc4279ba4c49af9 |
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| 出典メモ | uspto-grants-1980_06 |
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