反应详情

温度

145 °C

To a solution of N-(2-hydroxy-4-methoxyphenyl)-2-bromo-5-methyl-3-thiophenecarboxamide (2.1 g) in dimethyl sulfoxide (17 ml) was added potassium carbonate (1.7 g), and the mixture was stirred at 145° C. for 2 hours. The reaction system was cooled to room temperature and the reaction mixture was poured into ice water. The precipitated crystals were collected by filtration and the obtained crystals were purified by silica gel column chromatography (chloroform:methanol=20:0-20:1). The obtained solid was collected by filtration from diisopropyl ether-ethyl acetate-methanol to give 8-methoxy-2-methylthieno[2,3-b][1,5]benzoxazepin-4(5H)-one (530 mg).

1. temperatureThe reaction system was cooled to room temperature
2. filtrationThe precipitated crystals were collected by filtration
3. customthe obtained crystals were purified by silica gel column chromatography (chloroform:methanol=20:0-20:1)
4. filtrationThe obtained solid was collected by filtration from diisopropyl ether-ethyl acetate-methanol