Bromine → HCID 25130824, compound

Participants

Reaction Steps

Compound 14z (0.53 g, 1.99 mmol; HBr form) in acetic acid (2 mL) was treated dropwise with bromine (103 μL, 1.99 mmol), and the reaction mixture was stirred at room temperature for 3 h. The white precipitate was collected by filtration and washed with cold acetone to yield 15z as a white powder (0.59 g, 86%). Mp decomposition at 122° C. 1H NMR (600 MHz, DMSO-d6): δ 4.99 (q, J=6 Hz, 1H), 2.88 (q, J=6 Hz, 2H), 1.69 (d, J=6 Hz, 3H), 1.16 (t, J=6 Hz, 3H). 13C NMR (150 MHz, DMSO-d6): δ 185.5, 170.7, 115.5×2, 47.6, 47.5, 24.0, 20.8, 13.5. MS m/z (ESI) 263.00 [M+H]+, 264.96 [(M+2)+H]+.

Provenance & Evidence