反应详情

温度

70 °C

A mixture of 3-amino-5-(pyridin-4-yl)thiophene-2-carboxamide (0.108 g, 0.500 mmol), 2-butanone (1.0 mL), p-toluenesulfonic acid monohydrate (0.0096 g, 0.050 mmol) and acetic acid (3.0 mL) was stirred for 1 h at 70° C. The reaction mixture was poured into aqueous sodium hydrogen carbonate (200 mL). Extraction with ethyl acetate (200 mL, 100 mL), washing with aqueous sodium hydrogen carbonate, drying over magnesium sulfate, filtration and concentration at reduced pressure gave a residue, which was triturated with dichloromethane/ethyl acetate (1:1, 6 mL), and the precipitate was collected by filtration to afford the title compound (0.095 g, 69%) as a yellow solid:

1. extractionExtraction with ethyl acetate (200 mL, 100 mL)
2. washwashing with aqueous sodium hydrogen carbonate
3. dry with materialdrying over magnesium sulfate, filtration and concentration at reduced pressure
4. customgave a residue, which
5. customwas triturated with dichloromethane/ethyl acetate (1:1, 6 mL)
6. filtrationthe precipitate was collected by filtration