Thionyl Chloride → HCID 14067389, Verbindung

HRID 614525Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 614525
[CH:1]1[N:9]2[C:4]([CH2:5][O:6][C:7]3[CH:13]=[CH:12][CH:11]=[CH:10][C:8]=32)=[N:3][C:2]=1[C:14]([OH:16])=O.S(Cl)([Cl:19])=O>>[CH:1]1[N:9]2[C:4]([CH2:5][O:6][C:7]3[CH:13]=[CH:12][CH:11]=[CH:10][C:8]=32)=[N:3][C:2]=1[C:14]([Cl:19])=[O:16]

Komponenten

3

Edukt 2

HCID 24386Thionyl ChlorideHCID 12909281HCID 12909281, Verbindung

Produkt 1

HCID 14067389HCID 14067389, VerbindungAusbeute 83 %

Versuchsvorschrift

5 g (0.023 mole) of 4H-imidazo-[2,1-c][1,4]-benzoxazine-2-carboxylic acid were suspended in 15 ml of thionyl chloride and the mixture obtained was refluxed for two hours during which time the solid material completely dissolved. Excess thionyl chloride was removed by azeotroping with benzene on a rotary evaporator and the product was triturated with ether, filtered off and dried to obtain 4.5 g (83% yield of 4H-imidazo-[2,1-c][1,4]-benzoxazine-2-carbonyl chloride with a melting point of 240° C. (decomp).

Aufarbeitung

  1. customthe mixture obtained
  2. temperaturewas refluxed for two hours during which time the solid material
  3. dissolutioncompletely dissolved
  4. customExcess thionyl chloride was removed
  5. customby azeotroping with benzene on a rotary evaporator
  6. customthe product was triturated with ether
  7. filtrationfiltered off
  8. customdried

Quellen und Nachweise

ORD-Eintrag
ord-de8aacaa292e44b69b6f78b94c6a08d3
Quelldatensatz
uspto-grants-1979_03
Patentnummer
US04145419

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