反应详情

To a solution of 0.235 g acetic acid 2-(3-methyl-5-sulfamoyl-thiophen-2-yl)-ethyl ester in 5 ml acetonitrile was added 0.188 g phenylchloroformate and 0.252 g triethylamine at 0° C. and the mixture was stirred at this temperature for 2 h. To the resulting suspension was added 0.220 g 6-methyl-4-trifluoromethyl-pyridin-2-ylamine and the mixture was heated to 60C for 18 h. The reaction mixture was partitioned between 10% citric acid and ethyl acetate. The phases were separated and the organic phase was washed with brine and evaporated. The residue was triturated with diethylether. The solid was collected by filtration to yield 0.736 g of the title compound as light yellow crystals. MS (ISN) M−H+=463.9

1. customThe reaction mixture was partitioned between 10% citric acid and ethyl acetate
2. customThe phases were separated
3. washthe organic phase was washed with brine
4. customevaporated
5. customThe residue was triturated with diethylether
6. filtrationThe solid was collected by filtration