反应详情

To a solution of 4-(2,3-dichlorobenzyl)-2-(methylthio)thiazolo[4,5-d]pyrimidin-7(4H)-one (660 mg, 1.842 mmol) in THF (150 mL) and water (60 mL) at 0-5° C. was added Oxone (6.8 g, 11.05 mmol). The resulting mixture was stirred at ambient temperature for 60 hours. After removing THF under reduced pressure, the precipitate formed was collected by filtration and the precipitate was further washed with water, ether and dried in vacuo to give the desired product as a white solid (574 mg, 80%). The compound was directly used in next step without further purification. 1H NMR (300 MHz, CDCl3) δ 8.53 (br, 1H), 7.54 (dd, J=7.8, 1.5 Hz, 1H), 7.35˜7.24 (m, 2H), 5.61 (s, 2H), 3.33 (s, 3H); LC-MS: 390 (MH+); IR (thin film): 3027, 3008, 2925, 1649, 1602, 1488, 1461, 1424, 1405, 1335 cm−1.

1. customAfter removing THF under reduced pressure
2. customthe precipitate formed
3. filtrationwas collected by filtration
4. washthe precipitate was further washed with water, ether
5. customdried in vacuo