HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Ethyl cyanoacetate → HCID 178507928, Verbindung
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Ethyl cyanoacetate | HCID 7764 | — |
| Edukt | Benzenamine, 4-methylbenzenesulfonate (1:1) | HCID 84165 | — |
| Produkt | HCID 178507928 | HCID 178507928 | — |
Reaktionsschritte
The appropriate aniline p-toluenesulfonate and ethyl cyanoacetate are combined in equimolar quantities and heated at 225° to 260° C. until a melt required. (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 1 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 1 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.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US04031217 |
| Quelldatensatz | uspto-grants-1977_06 |
| ORD ID | ord-16b1288da846456487d781eef8eca753 |
| Quellennotiz | uspto-grants-1977_06 |