Water → 7-Iodo-1H-benzo[d][1,3]oxazine-2,4-dione

HRID 1449567

Reaktionsgleichung

Reaktionsgleichung von HRID 1449567
[I:1][C:2]1[CH:10]=[C:9]2[C:5]([C:6](=[O:12])[C:7](=[O:11])[NH:8]2)=[CH:4][CH:3]=1.[OH2:13]>C(O)(=O)C.C(OC(=O)C)(=O)C.[O-2].[O-2].[O-2].[Cr+6]>[I:1][C:2]1[CH:3]=[CH:4][C:5]2[C:6](=[O:12])[O:11][C:7](=[O:13])[NH:8][C:9]=2[CH:10]=1

Komponenten

6

Edukt 2

HCID 962WaterHCID 143872746-iodo-2,3-dihydro-1H-indole-2,3-dione

Produkt 1

HCID 189299207-Iodo-1H-benzo[d][1,3]oxazine-2,4-dioneAusbeute 81,8 %

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 10219390chromium (VI) trioxideKatalysatorHCID 176Acetic AcidLösungsmittelHCID 7918Acetic AnhydrideLösungsmittel

Reaktionsbedingungen

Temperatur
80 °C

Versuchsvorschrift

To a stirred warm (80° C.) solution of 6-iodo-1H-indole-2,3dione (3.0 g, 11 mM) in acetic acid (10 mL) and acetic anhydride (10 mL) was added in small portions chromium trioxide (1.83 g, 18.3 mM) while maintaining the temperature of the reaction mixture at 80°-90° C. The reaction mixture was then heated at 80° C. for 10 min, cooled and poured into water. The resulting mixture was filtered and the collected solids dried to provide the title compound as a yellow solid (2.6 g, 81.8%); MS(CI): 290 (M+H).

Aufarbeitung

  1. temperaturewhile maintaining the temperature of the reaction mixture at 80°-90° C
  2. temperaturecooled
  3. filtrationThe resulting mixture was filtered
  4. customthe collected solids dried

Quellen und Nachweise

ORD-Eintrag
ord-538c5ab905094dd6a93d5d5fdc38ecb0
Quelldatensatz
uspto-grants-1997_02
Patentnummer
US05599814

Verknüpfte Notizen

Wird geladen…