反应详情

4-Amino-N-methylbenzenesulfonamide (244 mg, 1.31 mmol) was dissolved in tetrahydrofuran (12 ml) and triethylamine (402 μl, 2.88 mmol) was added. Then a solution of 4,6-dichloropyrimidine-5-carbonyl chloride (300 mg, 1.42 mmol, prepared according to E. V. Tarasov et al. Synlett 2000, 5, 625-626) was dropwise added. After 2 h more triethylamine (202 μl, 1.44 mmol) and 4,6-dichloropyrimidine-5-carbonyl chloride (150 mg, 0.71 mmol) were added. The reaction mixture was stirred at room temperature overnight. The reaction mixture was then diluted with dichloromethane, washed with 4% sodium bicarbonate solution, dried over magnesium sulphate, filtered and evaporated. The crude was purified by flash chromatography (0% to 60%, hexane-ethyl acetate) using a SP1® Purification System to give 238 mg (50% yield) of the title compound. Purity 100%.

1. washwashed with 4% sodium bicarbonate solution
2. dry with materialdried over magnesium sulphate
3. filtrationfiltered
4. customevaporated
5. customThe crude was purified by flash chromatography (0% to 60%, hexane-ethyl acetate)
6. customa SP1® Purification System