HCID 71062618, compound → HCID 71063083, compound

Participants

Reaction Steps

Aqueous HBr (100 mL) was added to 1D (10 g, 29 mmol), and the reaction mixture was refluxed overnight. The reaction mixture was then brought to room temperature and extracted with ethyl acetate (2×100 mL). The organic layer was dried over sodium sulfate and filtered. The filtrate was removed under reduced pressure to afford crude compound (8 g) as a solid, which was carried on to the next step without further purification. 1H NMR (400 MHz, DMSO-d6): δ 12.4 (s, 1H), 10.4 (s, 1H), 7.76 (d, J=8.0 Hz, 1H), 6.75 (dd, J1=2.4 Hz, J2=8.8 Hz, 1H), 6.64 (d, J=2.4 Hz, 1H), 3.0-2.85 (m, 3H), 2.73 (d, J=16.4 Hz, 1H), 2.7-2.61 (m, 1H), 2.48 (m, 1H), 2.38 (m, 1H), 2.11 (m, 1H). ESI-MS m/z: 301 (M−H)−.

Provenance & Evidence