Ethyl cyanoacetate → HCID 54413059, Verbindung

HRID 1704729

Reaktionsgleichung

Reaktionsgleichung von HRID 1704729
CC[O-].[Na+].[C:5]([CH2:7][C:8](OCC)=[O:9])#[N:6].[C:13]1([CH:19]=[C:20]2[C:25](=[O:26])[C:24](=[CH:27][C:28]3[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=3)[CH2:23][S:22][CH2:21]2)[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1>CCO>[O:9]=[C:8]1[O:26][C:25]2[C:24](=[CH:27][C:28]3[CH:29]=[CH:30][CH:31]=[CH:32][CH:33]=3)[CH2:23][S:22][CH2:21][C:20]=2[CH:19]([C:13]2[CH:14]=[CH:15][CH:16]=[CH:17][CH:18]=2)[CH:7]1[C:5]#[N:6]

Komponenten

5

Edukt 3

HCID 7764Ethyl cyanoacetateHCID 336779tetrahydro-3,5-bis(phenylmethylene)-4H-thiopyran-4-oneHCID 2723922Sodium ethoxide

Produkt 1

HCID 54413059HCID 54413059, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel2×

Versuchsvorschrift

To a solution of NaOEt (from 555 mg, 92 mg atom Na in absolute EtOH) in 100 ml of absolute EtOH is added ethyl cyanoacetate (2.44 g, 22 mmole) dissolved in 50 ml of absolute EtOH. This is heated at reflux temperature for 2 hours, cooled slightly and tetrahydro-3,5-bis(phenylmethylene)-4H-thiopyran-4-one (5.84 g, 20 mmole) is added at once. The mixture quickly turns orange-red for ca. 10 minutes, changing to yellow (yellow solids in orange-red solution) as heating is continued for 2 hours.

Aufarbeitung

  1. temperatureThis is heated
  2. temperatureat reflux temperature for 2 hours
  3. temperaturecooled slightly
  4. temperatureas heating
  5. waitis continued for 2 hours

Quellen und Nachweise

ORD-Eintrag
ord-b0cd7425e0bf47af9e85693cd6ceaf55
Quelldatensatz
uspto-grants-1978_11
Patentnummer
US04127667

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