反应详情

To a solution of diethyl 3-((4-hydroxy-2-(pyridin-2-yl)pyrimidine-5-carboxamido)(4-methoxyphenyl)methyl)phenylphosphonate, 5-e, (0.99 g, 1.81 mmol) in dichloromethane (20 ml) was added TMSBr (5.6 g, 36.2 mmol) dropwise at 0° C. The resulting mixture was stirred at room temperature for 2 days. Then it was concentrated under vacuum and the residue was purified on prep-HPLC to provide the product, 5-1, (400 mg, 45%). 1H NMR (DMSO-d6, 300 MHz,): δ 8.80-8.82 (m, 1H), 8.37-8.40 (m, 1H,), 8.07-8.12 (m, 1H), 7.70-7.74 (m, 1H), 7.52-7.64 (m, 2H), 7.38-7.43 (m, 2H), 7.23-7.25 (m, 2H), 6.92-6.95 (m, 2H), 6.25-6.28 (m, 1H), 3.73 (s, 3H). (M−H)−=491.1.

1. concentrationThen it was concentrated under vacuum
2. customthe residue was purified on prep-HPLC
3. customto provide the product, 5-1, (400 mg, 45%)