反应详情

温度

110 °C

The neat reaction of 4-methyl-5-(hydroxymethyl)thiazole (590 mg, 4.57 mmol) and 2-chloroacetophenone (710 mg, 4.59 mmol) was heated at 110° C. The mixture solidified within 15 minutes. Acetonitrile (10 mL) was added and the mixture refluxed for another 3 hrs. It was cooled to room temperature and tert-butyl methyl ether (5 mL) was added and the reaction mixture was left overnight at room temperature. The product crystallized was filtered and washed well with a mixture of hexanes:EtOAc (1:1, v/v) and dried. It was recrystallized from a mixture of actonitrile/ethanol/tert-butyl methyl ether; yield 130 mg (10%); mp. 240–242° C. (dec.).

1. temperaturethe mixture refluxed for another 3 hrs
2. temperatureIt was cooled to room temperature
3. waitthe reaction mixture was left overnight at room temperature
4. customThe product crystallized
5. filtrationwas filtered
6. washwashed well with a mixture of hexanes:EtOAc (1:1
7. customv/v) and dried
8. customIt was recrystallized from a mixture of actonitrile/ethanol/tert-butyl methyl ether