反应详情

To a solution of ethyl phosphate (1-1-1, 260 mg, 0.47 mmol) in dichloromethane (10 ml) was added TMSBr (2.18 g, 14.2 mmol) dropwise at 0° C. The resulting mixture was stirred at room temperature for 3 days. The mixture was concentrated under vacuum and methanol (20 ml) was added. The mixture was stirred for 15 mins at room temperature and concentrated. The residue was purified on prep-HPLC to provide the product, 1-1-2. (100 mg, 43%). 1H NMR (DMSO-d6, 300 MHz,): δ 8.81 (d, 1H, J=6 Hz), 8.40 (m, 1H), 8.10 (m, 1H), 7.60 (m, 4H), 7.35 (m, 2H), 7.25 (m, 2H), 6.95 (m, 2H), 6.23 (d, 1H, J=6 Hz), 3.71 (s, 3H). (M−H)−=491.1.

1. concentrationThe mixture was concentrated under vacuum and methanol (20 ml)
2. additionwas added
3. stirringThe mixture was stirred for 15 mins at room temperature
4. concentrationconcentrated
5. customThe residue was purified on prep-HPLC
6. customto provide the product, 1-1-2