反应详情

温度

60 °C

Sodium hydride (440 mg) was suspended in dimethylformamide (10 ml), and 1,2,4-triazole (948 mg) was added to the suspension, to which a solution of 1-(2,4-difluorophenyl)-1-(6-cyanobenzothiazol-2-yl)-2-chloroethanol (1.49 g) in dimethylformamide (10 ml) was added. The mixture was heated at 60° C. for 4 hours. After the liquid reaction mixture was cooled to room temperature, ethyl acetate and water were added thereto. An organic layer separated was washed three times with water and then dried over magnesium sulfate, and the solvent was distilled out. The residue was recrystallized from dichloromethanediisopropyl ether to obtain the intended compound (1.17 g). Melting point: 170°-172° C.

1. additionwas added
2. customAfter the liquid reaction mixture
3. temperaturewas cooled to room temperature
4. customAn organic layer separated
5. washwas washed three times with water
6. dry with materialdried over magnesium sulfate
7. distillationthe solvent was distilled out
8. customThe residue was recrystallized from dichloromethanediisopropyl ether