反应详情

温度

50 °C

A 5-mL reaction vial with a stirring vane and a teflon cap was charged with 3,3′,4,4′-tetrahydroxybenzil (137 mg; 0.500 mmol) and 1.00 mL of m-cresol (Acros) which gives a yellow-brown slurry warming to ca. 50° C. The suspension is treated with sulfate 5,6-diamino-2,4-dihydroxypyrimidine sulfate (120 mg; 0.500 mmol; 1.00 equiv) which is insoluble in the reaction solution at room temperature and goes into solution on heating to ca. 200° C. to give homogeneous dark solution. Heating between 200° C. and 220° C. for an additional 2 h, followed by cooling to room temperature, and precipitation by pouring into 40 mL of anhydrous diethyl ether resulted in a light yellow precipitate. The solid was centrifuged, the supernatant decanted, the solid precipitate was washed with 4×40 mL of diethyl ether and dried in a vacuum dessicator to yield a yellow solid. MS (M+H+: calcd 381; found 381).

1. customA 5-mL reaction vial with a stirring vane
2. customgives a yellow-brown slurry
3. customis insoluble in the reaction solution at room temperature
4. temperatureon heating to ca. 200° C.
5. customto give homogeneous dark solution
6. temperatureHeating between 200° C. and 220° C. for an additional 2 h
7. temperatureby cooling to room temperature
8. customprecipitation
9. additionby pouring into 40 mL of anhydrous diethyl ether
10. customresulted in a light yellow precipitate
11. washthe supernatant decanted, the solid precipitate was washed with 4×40 mL of diethyl ether
12. customdried in a vacuum dessicator
13. customto yield a yellow solid