反应详情

To a stirred solution of 2-[3,5-dichloro-4-(3-amino-4-methoxy-phenoxy)-phenyl]-2H-[1,2,4]triazine-3,5-dione (100 mg) in pyridine (1 mL) was added 4-fluorobenzenesulfonyl chloride (59 mg) and the resulting solution was allowed to stir at room temperature for 1 h. The reaction solution was poured over water, extracted with ethyl acetate, the organic layer washed with 1N hydrochloric acid, water, brine, dried (Na2SO4), concentrated in vacuo and flash chromatographed on silica gel (40% acetone/hexanes) to afford the title compound of Step B as a light-yellow colored solid, 115 mg. m.p. 90-96° C., MS Calc.:553.4; Found:550.9.

1. extractionextracted with ethyl acetate
2. washthe organic layer washed with 1N hydrochloric acid, water, brine
3. dry with materialdried (Na2SO4)
4. concentrationconcentrated in vacuo and flash
5. customchromatographed on silica gel (40% acetone/hexanes)