反应详情

A solution of 2-[3,5-dichloro-4-(4-methoxy-phenoxy)-phenyl]-2H-[1,2,4]triazine-3,5-dione (1 g) and hexamethylenetetraamine (0.6 g) in trifluoroacetic acid (8 mL) was stirred at 70° C. for 18 h. The trifluoroacetic acid was removed in vacuo, water added and the resulting mixture was stirred for 30 min. The residue was extracted with ethyl acetate, the organic phase washed with water, brine, dried (Na2SO4), concentrated in vacuo and flash chromatographed on silica gel (35% acetone/hexanes) to afford the title compound of Step A as an off-white solid, 1.0 g (m.p. 184-187° C.).

1. customThe trifluoroacetic acid was removed in vacuo, water
2. additionadded
3. extractionThe residue was extracted with ethyl acetate
4. washthe organic phase washed with water, brine
5. dry with materialdried (Na2SO4)
6. concentrationconcentrated in vacuo and flash
7. customchromatographed on silica gel (35% acetone/hexanes)