Reaktion #521398

ord-27427512053c4a09b794d01d097195cb

Lösungsmittel

Reaktionsbedingungen

Temperatur
30°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    FiltrationFor work-up, the solid is filtered off with suction
  2. 2
    workup.ADDITIONthe filtrate is diluted with methylene chloride
  3. 3
    Extraktionextracted with water
  4. 4
    Waschenwashed twice with water
  5. 5
    SonstigeThe organic phase is dried
  6. 6
    Einengenconcentrated

Vorschrift

30 g (170 mmol) of 2-(4,5-dihydroisoxazol-3-yl)-3-methylaniline are dissolved in 400 ml of acetonitrile, and 94 g (0.68 mol) of potassium carbonate are added. 84 g (174 mmol) of tetrabutylammonium tribromide are subsequently added a little at a time with vigorous stirring at temperatures<30° C. For work-up, the solid is filtered off with suction and the filtrate is diluted with methylene chloride and extracted with water. The solvent is stripped off and the residue is again taken up in methyl tert-butyl ether and washed twice with water. The organic phase is dried and concentrated.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06670482B2uspto-grants-2003_12