反应详情

A solution of methylurea (148 mg; 2.0 mmoles) in DMF (2 ml) was cooled to 0° C., and α-trifluoromethylacryloyl chloride (317 mg; 2.0 mmoles) was added dropwise. The mixture was stirred at room temperature for 1 hour, and water (20 ml) was added. The mixture was extracted with methylene chloride (20 ml×1, 10 ml×2). The combined extracts were dried over anhydrous magnesium sulfate, filtered, and concentrated under reduced pressure. The residue was purified by a column chromatography on silica gel (chloroform:ethyl acetate=3:1) to give 39 mg (yield: 10%) of 1-methyl-5-trifluoromethyl-5,6-dihydrouracil (OF-3) and 117 mg (yield: 30%) of 3-methyl-5-trifluoromethyl-5,6-dihydrouracil (OF-2).

1. extractionThe mixture was extracted with methylene chloride (20 ml×1, 10 ml×2)
2. dry with materialThe combined extracts were dried over anhydrous magnesium sulfate
3. filtrationfiltered
4. concentrationconcentrated under reduced pressure
5. customThe residue was purified by a column chromatography on silica gel (chloroform:ethyl acetate=3:1)