反应详情

5-Hydroxy-6-methoxy-4-nitro-isobenzofuran-1,3-dione (115 mg), aluminum chloride (80 mg) was mixed with ethyl acetate (3 ml). Pyridine (155 μl) in ethyl acetate (2 ml) was added dropwise. The resulting mixture was stirred at room temperature for 0.5 hours, heated to reflux for 3 hours, and then quenched with water (0.5 ml) and conc. HCl (0.5 ml) at 60° C. Ethyl acetate and water was removed in vacuo. The remainder was mixed with brine (2 ml) and extracted two times with ethyl acetate (15 ml). The combined organic layers were dried over anhydrous Na2SO4, filtrated, evaporated and triturated with diethyl ether.

1. temperatureheated
2. temperatureto reflux for 3 hours
3. customquenched with water (0.5 ml) and conc. HCl (0.5 ml) at 60° C
4. customEthyl acetate and water was removed in vacuo
5. additionThe remainder was mixed with brine (2 ml)
6. extractionextracted two times with ethyl acetate (15 ml)
7. dry with materialThe combined organic layers were dried over anhydrous Na2SO4
8. filtrationfiltrated
9. customevaporated
10. customtriturated with diethyl ether