反应详情

温度

70 °C

A mixture of 3-(butylamino)-5-(pyridin-4-yl)thiophene-2-carboxamide (0.100 g, 0.400 mmol), acetone (3.0 mL), p-toluenesulfonic acid monohydrate (0.0095 g, 0.050 mmol) and acetic acid (2.0 mL) was stirred for 3 days at 70° C. in a sealed tube. The mixture was poured into sat. aqueous sodium hydrogen carbonate (100 mL). Extraction with ethyl acetate-tetrahydrofuran (2:1, 100 mL), drying over magnesium sulfate, filtration and concentration at reduced pressure gave an oil. The oil was purified by column chromatography (Combiflash, 12 g silica gel, hexane to ethyl acetate) to afford the title compound (0.0879 g, 70%) as a yellow solid:

1. extractionExtraction with ethyl acetate-tetrahydrofuran (2:1, 100 mL)
2. dry with materialdrying over magnesium sulfate, filtration and concentration at reduced pressure
3. customgave an oil
4. customThe oil was purified by column chromatography (Combiflash, 12 g silica gel, hexane to ethyl acetate)