Reaktion #50002

ord-87571bf49b2c43568c8a92beb534f448

Reaktionsbedingungen

Temperatur
0°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.ADDITIONTo this was added very slowly
  2. 2
    Filtrationthe resulting crystals filtered off
  3. 3
    Waschenwashed with water until neutral and
  4. 4
    Sonstigedried in vacuo

Vorschrift

23.7 g 2,4-Dichloro-6-fluorobenzothiazole was dissolved in 100 ml concentrated sulfuric acid and the solution cooled to 0° C. To this was added very slowly, dropwise, a cooled solution of 14 ml concentrated sulfuric acid and 14 ml 100% nitric acid. The mixture was stirred for 3 hours, poured into 500 ml ice water, the resulting crystals filtered off, washed with water until neutral and dried in vacuo. Yield: 22.7 g=79% of theory m.p.: 110°-112° C.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05424443uspto-grants-1995_06