反应详情

A solution of 2-amino-5-fluoro pyridine (0.15 g, 1.38 mmol) in 10 ml dry dioxane was treated at 0° C. with trimethylaluminium (2M in hexane, 0.69 ml, 1.38 mmol). The mixture was stirred at room temperature for 1 h. 2-Methyl-5-(3-sulfamoyl-phenylamino)-thiazole-4-carboxylic acid ethyl ester (0.12 g, 0.35 mmol) was added and the reaction mixture was refluxed for 4 h. 1 ml water and 2 g sodium sulfate were sequentially added and filtered. The filtrate was evaporated and the residue purified by flash chromatography (hetane, ethyl acetate) to yield 2-methyl-5-(3-sulfamoyl-phenylamino)-thiazole-4-carboxylic acid (5-fluoro-pyridin-2-yl)-amide (0.004 g, 3%) as an off-white solid, MS (ISP): m/e=408.4 (M+H+).

1. temperaturethe reaction mixture was refluxed for 4 h
2. filtrationfiltered
3. customThe filtrate was evaporated
4. customthe residue purified by flash chromatography (hetane, ethyl acetate)