反应详情

Red fuming nitric acid (10 mL) was added to a stirred suspension of 6-Chloro-4-hydroxy-chromen-2-one (2.0 g, 10.17 mmol) in chloroform (200 mL) at 0° C. The resultant solution was stirred at 0° C. for 1.5 h, quenched with water (80 mL), the organics separated and treated with saturated NaHCO3 when a thick yellow solid fell out of solution. The solid was filtered and the filtrate acidified with 3N HCl (pH 2) and extracted with chloroform. The organic extracts were dried to a yellow powder and all solids were combined and identified as 6-chloro-4-hydroxy-3-nitro-chromen-2-one. 1H NMR (300 MHz, DMSO-d6) δ ppm 7.78 (d, 1H), 7.55 (dd, 1H), 7.23 (d, 1H).

1. customquenched with water (80 mL)
2. customthe organics separated
3. additiontreated with saturated NaHCO3 when a thick yellow solid
4. filtrationThe solid was filtered
5. extractionextracted with chloroform
6. customThe organic extracts were dried to a yellow powder