反应详情

The 4-(6,7-dimethoxyquinolin-4-yloxy)phenylamine (296 mg, 1.00 mmol) obtained by the method described in WO97/17329 and (3-methanesulfonylphenyl)carbamic acid phenyl ester (291 mg, 1.00 mmol) were heated and stirred in dimethylsulfoxide (3 ml) at 85° C. for 2 hours. The reaction solution was distributed between ethyl acetate and water, the organic layer was washed with 1N aqueous sodium hydroxide, water and saturated brine and dried over anhydrous magnesium sulfate, the drying agent was filtered off and the filtrate was distilled off under reduced pressure. The obtained crude product was subjected to silica gel column chromatography (eluent-ethyl acetate:methanol=30:1), the fraction containing the target substance was concentrated and suspended in ethyl acetate, the suspension was diluted with hexane and the crystals were filtered out, washed with hexane and blow-dried to obtain the title compound (430 mg, 0.871 mmol, 87%) as colorless crystals.

1. temperaturewere heated
2. washthe organic layer was washed with 1N aqueous sodium hydroxide, water and saturated brine
3. dry with materialdried over anhydrous magnesium sulfate
4. filtrationthe drying agent was filtered off
5. distillationthe filtrate was distilled off under reduced pressure
6. customThe obtained crude product
7. additionthe fraction containing the target substance
8. concentrationwas concentrated
9. additionthe suspension was diluted with hexane
10. filtrationthe crystals were filtered out
11. washwashed with hexane
12. customblow-dried