Reaktion #484329

ord-48185009ba5b4fda8f47291661fc6cdc

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    FiltrationFor work-up, the solid is filtered off with suction
  2. 2
    workup.ADDITIONthe solution 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. At temperatures <30° C., 84 g (174 mmol) of tetrabutylammonium tribromide are then added a little at a time, with vigorous stirring. For work-up, the solid is filtered off with suction and the solution is diluted with methylene chloride and extracted with water. The solvent is stripped off and the residue is then taken up again 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: US06608209B2uspto-grants-2003_08