関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Acetamidomalonic acid diethyl ester | HCID 14041 | — |
| 反応物 | Sodium | HCID 5360545 | — |
| 反応物 | 2-(Chloromethyl)-5-(4-nitrophenyl)furan | HCID 15212084 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | Diethyl acetamido[5-(4-nitrophenyl)furfuryl]malonate | HCID 53706585 | 50.2% |
反応手順
To 300 ml of absolute ethanol was added in portions 2.4 g (0.104 mole) of sodium followed by 21.7 g (0.10 mole) of diethyl acetamidomalonate and stirring was continued for 10 minutes. 5-(4-Nitrophenyl)furfuryl chloride (23.7 g, 0.10 mole) was then added in portions, and the mixture was heated under reflux for 5 hrs. The mixture was filtered hot to remove the insoluble sodium chloride. The filtrate was cooled in a refrigerator, and the solid which was deposited was collected by filtration and washed with ether. The solid was stirred in water, collected by filtration, and dried in an oven at 100° for 2 hrs. to give 21 g (50%) of diethyl acetamido[5-(4-nitrophenyl)furfuryl]malonate. Recrystallization from SDA-32 gave an analytical sample, m.p. 183°-185°.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04066669 |
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| 出典データセット | uspto-grants-1978_01 |
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| ORD ID | ord-c86a387e19df4205a3d015e04f3fad65 |
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| 出典メモ | uspto-grants-1978_01 |
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