Reaktion #322766

ord-e5c7fdf41bba45d78d36aa94385018c2

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigeat 0° to 5° C
  2. 2
    workup.ADDITIONpoured onto ice water
  3. 3
    FiltrationThe precipitated crystals were collected by filtration
  4. 4
    Waschenwashed with water
  5. 5
    Sonstigedried

Vorschrift

A solution of 7-fluoro-2H-1,4-benzoxazin-3(4H)-one (2.0 g) in 80% aqueous sulfuric acid (30 ml) was cooled to 0° to 5° C., and 60% nitric acid (1.6 g) was gradually added thereto at 0° to 5° C. The resultant mixture was stirred at the same temperature for 30 minutes and poured onto ice water. The precipitated crystals were collected by filtration, washed with water and dried to give 7-fluoro-6-nitro-2H-1,4-benzoxazin-3(4H)-one (2.1 g) as pale brown crystals. m.p., 205.9° C.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04640707uspto-grants-1987_02