Reaktion #350563

ord-e7557914f99c40acbe835f6180c02ff1

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturwas heated
  2. 2
    Temperaturat reflux for 17 h
  3. 3
    TemperaturThe reaction mixture was cooled
  4. 4
    Filtrationfiltered
  5. 5
    SonstigeThe filtrate was evaporated to dryness under reduced pressure

Vorschrift

A stirring mixture of 5-amino-2-chloro-4-fluorophenol (22.0 g, 136.19 mmol), 2-bromopropane (38.4 mL, 50.25 g, 408.57 mmol) and potassium carbonate (37.6 g, 273.0 mmol) was heated at reflux for 17 h. The reaction mixture was cooled and filtered. The filtrate was evaporated to dryness under reduced pressure. Flash chromatography yielded the title compound of Step A as a brown oil (17.2 g). 1H NMR (CDCl3): δ7.02 (d, 1H), 6.44 (d, 1H) 4.38 (q, 1H), 3.81 (br s,2H), 1.33 (d,6H). IR (cm-1): 3378.4, 3475.6.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05643855uspto-grants-1997_07