反应详情

温度

110 °C

The neat mixture of 2-bromo-2′,4′-dihydroxyacetophenone (3 g, 13 mmol) and 4,5-dimethylthiazole (1.71 g, 13.3 mmol) was heated at 110° C. for 3 hrs. It was dissolved in acetonitrile (15 mL) and cooled to room temperature. Tert-butyl methyl ether (5 mL) was added and the reaction mixture kept at room temperature overnight. The product crystallized was filtered, washed well with a mixture of acetonitrile and tert-butyl methyl ether (1:1, v/v) and dried. It was recrystallized from a mixture of methanol and a few drops of water. Yield: 2.5 g (50%); mp. 257–260° C. (dec.).

1. temperaturecooled to room temperature
2. customThe product crystallized
3. filtrationwas filtered
4. washwashed well with a mixture of acetonitrile and tert-butyl methyl ether (1:1
5. customv/v) and dried
6. customIt was recrystallized from a mixture of methanol and a few drops of water