Hydrochloric Acid → HCID 178418396, Verbindung

HRID 1707680Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1707680
C(OC([NH:8][C:9]1[CH:14]=[CH:13][C:12]([CH:15]([C:18](=O)[CH3:19])[C:16]#[N:17])=[CH:11][CH:10]=1)=O)(C)(C)C.C(O)C.C(O[CH:27](OCC)[CH2:28][NH:29][NH2:30])C.[ClH:34]>O1CCOCC1.C(OCC)(=O)C>[ClH:34].[NH2:8][C:9]1[CH:10]=[CH:11][C:12]([C:15]2[C:18]([CH3:19])=[N:30][N:29]3[CH:28]=[CH:27][NH:17][C:16]=23)=[CH:13][CH:14]=1

Komponenten

7

Edukt 4

HCID 313Hydrochloric AcidHCID 702EthanolHCID 322952(2,2-Diethoxyethyl)hydrazineHCID 196943922-(4-t-Butoxycarbonylaminophenyl)-3-oxobutyronitrile

Produkt 1

HCID 178418396HCID 178418396, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 8857Ethyl AcetateLösungsmittelHCID 312751,4-DioxaneLösungsmittel

Versuchsvorschrift

A mixture of 2.5 g of 2-(4-t-butoxycarbonylaminophenyl)-3-oxobutyronitrile, 20 ml of ethanol and 1.4 g of 2,2-diethoxyethylhydrazine was heated under reflux for 2 hours. 20 ml of 4N hydrogen chloride in dioxane were added, and then the whole mixture was heated under reflux for a further 30 minutes. After the mixture had been cooled, ethyl acetate was added to precipitate crystals. These crystals were collected by filtration and recrystallized from ethanol to give 1.4 g of the title compound as pale brown plates melting at 180°-190° C.

Aufarbeitung

  1. temperaturewas heated
  2. temperatureunder reflux for 2 hours
  3. temperaturethe whole mixture was heated
  4. temperatureunder reflux for a further 30 minutes
  5. temperatureAfter the mixture had been cooled
  6. customto precipitate crystals
  7. filtrationThese crystals were collected by filtration
  8. customrecrystallized from ethanol

Quellen und Nachweise

ORD-Eintrag
ord-e245fd82aa5f47a98801bd942a96736b
Quelldatensatz
uspto-grants-1994_10
Patentnummer
US05354768

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