反应详情

Sulphamoyl chloride solution in toluene (5 mL, 0.7 M, 3.5 mmol) was concentrated under reduced pressure (30° C. water bath temperature) to ca. 1 mL volume. The residue was cooled to 0° C. (ice bath) and N,N-dimethylacetamide (5 mL) was added. 4-{[Bis-(4-hydroxy-phenyl)-methyl]-[1,2,4]triazol-4-yl-amino}-benzonitrile (CAB2070, 250 mg, 0.65 mmol) was added to the colourless solution and the mixture was stirred for 18 h at, room temperature. Ethyl acetate (50 mL) and water (30 mL) were added to the solution, the organic layer was separated, washed with water (2×30 mL) and brine (20 mL), dried over sodium sulphate and concentrated under reduced pressure to give a white solid. The solid was dissolved in ethyl acetate and precipitated by addition of hexane. The white powder was filtered off and dried under high vacuum. Yield: 299 mg (85%).

1. additionwas added
2. customthe organic layer was separated
3. washwashed with water (2×30 mL) and brine (20 mL)
4. dry with materialdried over sodium sulphate
5. concentrationconcentrated under reduced pressure
6. customto give a white solid
7. customprecipitated by addition of hexane
8. filtrationThe white powder was filtered off
9. customdried under high vacuum