Phosphorus oxychloride → 6-Iodo-4-chloro-2-trichloromethyl quinazolin

HRID 2257509Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2257509
[I:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[NH:8][CH:7]([C:12]([Cl:15])([Cl:14])[Cl:13])[NH:6][C:5]2=O.O=P(Cl)(Cl)[Cl:19]>C1(C)C=CC=CC=1>[I:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[N:8]=[C:7]([C:12]([Cl:15])([Cl:14])[Cl:13])[N:6]=[C:5]2[Cl:19]

Komponenten

4

Edukt 2

HCID 24813Phosphorus oxychlorideHCID 190749436-Iodo-2-trichloromethyl-1,2-dihydro-quinazolin-4-one

Produkt 1

HCID 6329086-Iodo-4-chloro-2-trichloromethyl quinazolin

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1140TolueneLösungsmittel

Versuchsvorschrift

A suspension of 6-iodo-2-trichloromethyl-1,2-dihydro-quinazolin-4-one (38.9 g=100 mmol) in POCl3 (500 mL) was heated to reflux for 12 hours. The homogeneous solution was cooled and excess POCl3 was distilled under vacuum. Viscous oil obtained was poured over crushed ice and triturated vigorously to give grey solid, which was dissolved in toluene (200 mL), filtered and evaporated under vacuo to give off-white crystalline solid. Mp 154°-155° C. Elemental Analysis: Calculated for C9H3Cl4IN2, C: 26.50, H, 0.74, N: 6.87; Found: C: 26.15, H: 0.79, N. 6.68.

Aufarbeitung

  1. temperaturewas heated
  2. temperatureto reflux for 12 hours
  3. temperatureThe homogeneous solution was cooled
  4. distillationexcess POCl3 was distilled under vacuum
  5. customViscous oil obtained
  6. additionwas poured
  7. customover crushed ice
  8. customtriturated vigorously
  9. customto give grey solid, which
  10. filtrationfiltered
  11. customevaporated under vacuo
  12. customto give off-white crystalline solid

Quellen und Nachweise

ORD-Eintrag
ord-25c0ebfdce6146d4b0a6d1c12dbdd05f
Quelldatensatz
uspto-grants-1997_08
Patentnummer
US05658902

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