反应详情

温度

0 °C

To a solution of 4.00 g 6-acetyl-2-butyl-4-(1H)-quinazolinone in 250 ml of dry tetrahydrofuran, cooled to 0° C., is added dropwise 16.4 ml of 3.0M methylmagnesium bromide in diethyl ether. The reaction is stirred at 0° C. for 0.5 hours and then allowed to warm to room temperature followed by quenching with 100 ml of saturated ammonium chloride solution. The mixture is diluted with 50 ml of water and extracted with ethyl acetate. The combined organic layers are washed with brine, dried over anhydrous magnesium sulfate, filtered and concentrated in vacuo. The residue is purified by flash chromatography on silica gel, eluting with 100:0.25 chloroform-methanol to give 2.75 g of the desired product as a white solid. CI MASS SPEC 261(MH+).

1. temperatureto warm to room temperature
2. customby quenching with 100 ml of saturated ammonium chloride solution
3. additionThe mixture is diluted with 50 ml of water
4. extractionextracted with ethyl acetate
5. washThe combined organic layers are washed with brine
6. dry with materialdried over anhydrous magnesium sulfate
7. filtrationfiltered
8. concentrationconcentrated in vacuo
9. customThe residue is purified by flash chromatography on silica gel
10. washeluting with 100:0.25 chloroform-methanol