Reaction #2146762

ord-fb3ec38cabbc4589a151f2ca6ca6887b

Conditions

Detailed conditions
See reaction.notes.procedure_details.

Workup

  1. 1
    Temperatureat reflux for 4 h
  2. 2
    workup.ADDITIONit was poured on ice
  3. 3
    ExtractionThe aqueous solution was extracted three times with dichloromethane
  4. 4
    DryingThe combined organic layers were dried with MgSO4
  5. 5
    Otherevaporated

Procedure

2.6 g (12.0 mmol) of 7-Chloro-6-fluoro-isoquinoline 2-oxide (4) were heated in 40 ml of POCl3 at reflux for 4 h. After the mixture has cooled down to room temperature, it was poured on ice. The aqueous solution was extracted three times with dichloromethane. The combined organic layers were dried with MgSO4 and evaporated to yield 2.91 g of the title compound, which was used without further purification. Rt=2.34 min (Method A). Detected mass: 216.0/218.0 (M+H+).

Source

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08278294B2uspto-grants-2012_10