反应详情

温度

60 °C

To a solution of 0.263 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 ° C. and the mixture was stirred at this temperature for 2 h. To the resulting suspension was added 0.220 g 6-amino-4-trifluoromethyl-pyridine-2-carboxylic acid methyl ester and the mixture was heated to 60° C. 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 t-butylmethylether. The solid was collected by filtration to yield 0.376 g of the title compound as white crystals. MS (ISN) M−H+=508.3

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 t-butylmethylether
6. filtrationThe solid was collected by filtration