反应详情

To a solution of 7-fluoro-6-(1-methoxycarbonyl-2-methyl-2-propenyloxycarbonylamino)-4-propargyl-2H-1,4-benzoxazin-3(4H)-one (10 g) in toluene (100 g), sodium methoxide was added in an amount of 0.05 equivalent to one equivalent of the benzoxazine. The resulting mixture was refluxed for 3 hours, cooled to room temperature, combined with water and extracted with ethyl acetate. The organic layer was washed with water three times, dried over magnesium sulfate and concentrated. The residue was purified by silica gel column chromatography using a mixture of hexane and ethyl acetate as the eluent to give Compound No. 9 (6.1 g). m.p., 194°-198° C.

1. temperatureThe resulting mixture was refluxed for 3 hours
2. extractionextracted with ethyl acetate
3. washThe organic layer was washed with water three times
4. dry with materialdried over magnesium sulfate
5. concentrationconcentrated
6. customThe residue was purified by silica gel column chromatography
7. additiona mixture of hexane and ethyl acetate as the eluent
8. customto give Compound No
9. customm.p., 194°-198° C.