Bromine → HCID 59218663, compound

Participants

Reaction Conditions

Reaction Steps

Bromine (0.54 mL, 10.43 mmol) was added slowly to a solution of Example 8A (2.0 g, 6.96 mmol) in acetic acid (20 mL) at r.t. The reaction was heated to 86° C. and stirred for 1 h. The cooled solution was quenched with sat. bisulfite solution and extracted with EtOAc. Organics were dried (MgSO4) and concentrated in vacuo to give 2.4 g (94%) of the title compound as an orange solid. 1H NMR (400 MHz, CDCl3): δ 8.64 (s, 1H), 8.50 (br s, 1H), 7.40-7.55 (m, 3H), 7.18-7.26 (m, 1H), 3.46 (d, 3H, J=4.8 Hz). MS (ES) [m+H] calc'd for C14H9N3O2BrCl, 366, 368, 370; found 366, 368, 370.

Provenance & Evidence