Water → HCID 13318203, Verbindung

HRID 485308Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 485308
[F:1][C:2]1([C:14]([O:16][CH2:17][CH3:18])=[O:15])[CH:7]([O:8]C(=O)C)[NH:6][C:5](=[O:12])[NH:4][C:3]1=[O:13].[CH:19](=[N:25]/O)\[C:20]1[O:24][CH:23]=[CH:22][CH:21]=1.C(N(CC)CC)C.O>N1C=CC=CC=1>[F:1][C:2]1([C:14]([O:16][CH2:17][CH3:18])=[O:15])[CH:7]([O:8]/[N:25]=[CH:19]/[C:20]2[O:24][CH:23]=[CH:22][CH:21]=2)[NH:6][C:5](=[O:12])[NH:4][C:3]1=[O:13]

Komponenten

6

Edukt 4

HCID 962WaterHCID 8471TriethylamineHCID 68712882-Furancarboxaldehyde, oximeHCID 12946261HCID 12946261, Verbindung

Produkt 1

HCID 13318203HCID 13318203, VerbindungAusbeute 52,4 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1049PyridineLösungsmittel

Versuchsvorschrift

In 20 ml of pyridine were dissolved 5.24 g (20 mmol) of ethyl 5-fluoro-6-acetoxy-1,2,3,4,5,6-hexahydro-2,4-dioxopyrimidine-5-carboxylate and 2.62 g (23.6 mmol) of (E)-furfuraldoxime, and 2.02 g (20 mmol) of triethylamine was added to the solution, followed by stirring at room temperature for 15 hours. The reaction solution was poured into 200 ml of ice-cooled water, and crystals precipitated were collected by filtration and washed with water. The crystals were dried under reduced pressure and recrystallized from ethanol to give 3.28 g of ethyl 5-fluoro-6-(E)-furfurylideneaminooxy-1,2,3,4,5,6-hexahydro-2,4-dioxopyrimidine-5-carboxylate. m.p. 189°-190° C.

Aufarbeitung

  1. additionwas added to the solution
  2. customprecipitated
  3. filtrationwere collected by filtration
  4. washwashed with water
  5. customThe crystals were dried under reduced pressure
  6. customrecrystallized from ethanol

Quellen und Nachweise

ORD-Eintrag
ord-3c8452c7d0924ecd81821c455b465346
Quelldatensatz
uspto-grants-1985_08
Patentnummer
US04536504

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