反应详情

To a solution of 1.20 g of 2-butyl-6-ethynyl-4(1H)-quinazolinone in 90 ml of acetic acid is added 0.45 g of mercuric sulfate, 0.9 ml of water and 0.3 ml of sulfuric acid. The reaction mixture is heated at reflux for 5 hours, cooled to room temperature and quenched with 150 ml of water. The resulting mixture is concentrated in vacuo, diluted with 150 ml of water and extracted with 6:1 chloroform-methanol. The combined organics are dried over magnesium sulfate, filtered and concentrated in vacuo. The residue is purified by flash chromatography on silica gel, eluting with 1:1 ethyl acetate-hexanes to give 0.67 g of the desired product as a white solid. CI MASS SPEC 245(MH+).

1. temperatureThe reaction mixture is heated
2. temperatureat reflux for 5 hours
3. customquenched with 150 ml of water
4. concentrationThe resulting mixture is concentrated in vacuo
5. additiondiluted with 150 ml of water
6. extractionextracted with 6:1 chloroform-methanol
7. dry with materialThe combined organics are dried over magnesium sulfate
8. filtrationfiltered
9. concentrationconcentrated in vacuo
10. customThe residue is purified by flash chromatography on silica gel
11. washeluting with 1:1 ethyl acetate-hexanes