Reaction #1563948

ord-3d933e5eb70c495192de08fb045150d6

Solvents

Conditions

Detailed conditions
See reaction.notes.procedure_details.

Workup

  1. 1
    FiltrationThe reaction mixture was filtered over celite bed
  2. 2
    Washwashed with methanol
  3. 3
    ConcentrationThe filtrate and the washings were concentrated under reduced pressure

Procedure

10% Pd/C (400 mg) was added to a solution of 7-fluoro-5-nitro-2,3-dihydrobenzo[b][1,4]dioxine (2.0 g, 10 mmol) in methanol (50 mL) and stirring was continued at 25° C. under H2 atmosphere for 3 h. The reaction mixture was filtered over celite bed and washed with methanol. The filtrate and the washings were concentrated under reduced pressure to afford 7-fluoro-2,3-dihydrobenzo[b][1,4]dioxin-5-amine (Int-52) as pale brown liquid. MS (ESI): m/z 170.1 (M+H).

Source

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09402833B2uspto-grants-2016_08