Water → HCID 15428837, Verbindung

HRID 1489030Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1489030
[Cl:1][C:2]1[N:11]=[C:10]([NH:12][NH:13][C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)[C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[N:3]=1.C(N(CC)C(C)C)(C)C.[C:29](Cl)(Cl)=[O:30].O>C1COCC1>[Cl:1][C:2]1[N:11]2[C:29](=[O:30])[N:13]([C:14]3[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=3)[N:12]=[C:10]2[C:9]2[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=2[N:3]=1

Komponenten

6

Edukt 4

HCID 962WaterHCID 6371PhosgeneHCID 81531DiisopropylethylamineHCID 154288362-Chloro-4-phenylhydrazinoquinazoline

Produkt 1

HCID 15428837HCID 15428837, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

To a mixture of 2-chloro-4-phenylhydrazinoquinazoline (2 g, 7.4 mmol) and N,N-diisopropylethylamine (2 ml, 11.4 mmol) in THF was added phosgene (6 ml, 20% in Toluene) slowly, then stirred for additional 5 min. The reaction mixture was poured into water and extracted with ethyl acetate (2×100 ml). The combined organic layers were washed with brine and dried over Na2SO4 and evaporated under reduced pressure. The residue was triturated with ethanol and filtered to afford 5-chloro-2-phenyl-1,2,4-triazolo[4,3-c]quinazolin-3-one (1.8 g) as a yellow solid. m.p. 167°-168° C.

Aufarbeitung

  1. extractionextracted with ethyl acetate (2×100 ml)
  2. washThe combined organic layers were washed with brine
  3. dry with materialdried over Na2SO4
  4. customevaporated under reduced pressure
  5. customThe residue was triturated with ethanol
  6. filtrationfiltered

Quellen und Nachweise

ORD-Eintrag
ord-ab3233eb6dd74e74b9fe14341621ecb7
Quelldatensatz
uspto-grants-1997_10
Patentnummer
US05677309

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