反应详情

A mixture of 3-bromo-5-(hydroxy(phenyl)methyl)pyridin-4-ol (2.55 g, 91 mmol), TFA (16 mL) and Et3SiH in CH2Cl2 (30 mL) at rt for 10 h. It was concentrated in vacuo and the residue was purified by flash column on silica gel eluting with hexane/EtOAc/MeOH//600:300:50 followed by hexane/EtOAc/MeOH//400:400:50:10 to obtain an impure product which was triturated with a small amount of MeOH and Et2O to obtain the desired product (255 mg, 10%) as a white solid. 1H NMR (DMSO-d6) δ 11.75 (br s, 1H), 8.13 (s, 1H), 7.54 (s, 1H), 7.26-7.14 (m, 5H), 2.49 (s, 2H).

1. concentrationIt was concentrated in vacuo
2. customthe residue was purified by flash column on silica gel eluting with hexane/EtOAc/MeOH//600:300:50
3. customto obtain an impure product which
4. customwas triturated with a small amount of MeOH and Et2O