反应详情

温度

45 °C

4-Hydroxy-5-isobutyryl-3-methyl-2-phenylthieno[2,3-b]pyridine (35 g), potassium carbonate (18.6 g) and N,N-dimethylformamide (280 ml) were mixed and 2,6-difluorobenzyl bromide (27.9 g) was added and the reaction mixture was stirred at 40 to 50° C. for 2 hours. The reaction mixture was treated dropwise with water (560 ml), and the mixture was stirred for 1 hour and then cooled on ice, and then stirred further for 1 hour. The crude crystal was recovered by a filtration, washed with water (about 1000 ml), dried in air, suspended in a 1:1 solvent mixture (250 ml) of ethyl acetate and diisopropylether, and then the mixture was stirred at room temperature for 1 hour, and then stirred with cooling on ice for 1 hour. The crystal obtained by a filtration was washed with the same solvent mixture (180 ml), dried in vacuo at 40° C. for 5 hours to obtain the title compound (46.53 g, 94.6%).

1. stirringthe mixture was stirred for 1 hour
2. temperaturecooled on ice
3. stirringstirred further for 1 hour
4. filtrationThe crude crystal was recovered by a filtration
5. washwashed with water (about 1000 ml)
6. customdried in air
7. stirringthe mixture was stirred at room temperature for 1 hour
8. stirringstirred
9. temperaturewith cooling on ice for 1 hour
10. customThe crystal obtained by a filtration
11. washwas washed with the same solvent mixture (180 ml)
12. customdried in vacuo at 40° C. for 5 hours