反应详情

A mixture of 1.85 g (4.46 mmol) of 3-[4-chloro-2-fluoro-5-(phenylmethoxy)phenyl]-6-(trifluoromethyl)-2,4(1H, 3H)-pyrimidinedione, 492 μL (5.20 mmol) of dimethylsulfate, and 749 mg (8.92 mmol) of sodium bicarbonate in 20 mL of acetone was warmed under reflux for 3 h. Evaporation removed the solvent to give a viscous residue. It was dissolved in 50 mL of ether and washed twice with 30 mL of water, dried (MgSO4) and concentrated in vacuo to give white solid which was flash chromatographed over silica gel, eluting with a 1:4 v:v mixture of ethyl acetate and hexane to give 1.19 g of the title compound as a white solid, m.p.: 145°-147° C.; 1H-NMR (CDCl3, 200 MHz) ppm 7.4 (m, 6H), 6.85 (d, 1H), 6.4 (s, 1H), 5.1 (s, 2H), 3.55 (s, 3H).

1. temperaturewas warmed
2. temperatureunder reflux for 3 h
3. customEvaporation
4. customremoved the solvent
5. customto give a viscous residue
6. washwashed twice with 30 mL of water
7. dry with materialdried (MgSO4)
8. concentrationconcentrated in vacuo
9. customto give white solid which
10. customchromatographed over silica gel
11. washeluting with a 1:4 v
12. additionv mixture of ethyl acetate and hexane