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Ethyl cyanoacetate → HCID 178507928、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethyl cyanoacetate | HCID 7764 | — |
| 反応物 | Benzenamine, 4-methylbenzenesulfonate (1:1) | HCID 84165 | — |
| 生成物 | HCID 178507928 | HCID 178507928 | — |
反応手順
The appropriate aniline p-toluenesulfonate and ethyl cyanoacetate are combined in equimolar quantities and heated at 225° to 260° C. until a melt resulted. (Higher temperatures are used if necessary to achieve a melt). The temperature of the melt is lowered to 240° to 250° C. and heating continued for one hour. The hot melt is poured into ice-cold chloroform (about 1 to 1.5 liters per mole of aniline reactant) and the mixture stirred for one hour. The solid is filtered off, added to water-ethanol (1 liter of 1:1 per mole of aniline reactant) at 45° to 50° C. and the solution made basic with ammonium hydroxide. The solid is separated by filtration and recrystallized from a suitable solvent such as isopropanol.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04014881 |
| 出典データセット | uspto-grants-1977_03 |
| ORD ID | ord-c41154695f164f138fff195b6dfe4258 |
| 出典メモ | uspto-grants-1977_03 |