Bromine → HCID 86698556, compound

Participants

Reaction Steps

The solid (10 g, 49.60 mmol) from step 1 dissolved in acetic acid (70 mL) was added with Br2 (12.7 mL, 247.93 mmol) dropwise for 2 h. Then the reaction mixture was kept stirring at rt for 5.5 h. The resulting mixture was poured to ice water (1 L) and quenched with excess of NaHSO3 until the solution became clear with yellow suspension. The quenched solution was filtered to get title compound (13.52 g, 97.2%). 1H NMR (400 MHz, DMSO-d6) δ 1.07 (t, J=7.6 Hz, 3H), 2.36 (q, J=7.6 Hz, 2H), 7.80 (d, J=7.6 Hz, 1H), 7.84 (d, J=8.8 Hz, 1H), 9.50 (br s, 1H); 13C NMR (100 MHz, DMSO-d6) δ 10.1, 29.3, 117.3, 117.4, 119.0, 119.2, 121.0, 121.2, 128.4, 134.45, 134.49, 153.4, 155.9, 173.0;

Provenance & Evidence