反应详情

温度

25 °C

To a mixture of 335 mg (1.89 mmol) of 11a in 4 mL of aqueous 0.1N H2SO4 was added dropwise 10 mL of aqueous 0.2M KIO4 (2 mmol) at 25° C. The mixture was stirred at 25° C. for 2 h, filtered and washed with water, dried to leave 222 mg (67%) of 12a as an almost colorless solid, mp>250° C. 1H NMR (DMSO-d6), 7.043 (d, 1, J=8.4), 7.089 (t, 1, J=7.8), 7.232 (s, 2), 7.577 (t, 1, J=7.8), 7.735 (d, 1, J=7.5), 10.735 (s, 1). 1H NMR (DMSO-d6 +D2O), 7.043 (d, 1), 7.098 (t, 1), 7.577 (t, 1), 7.735 (d, 1). MS, 175 (20, M+), 147 (20), 119 (100), 92 (60). High resolution MS, Calcd for C9H5NO3 175.0267, found 175.0275.

1. filtrationfiltered
2. washwashed with water
3. customdried