反应详情

The compound obtained in Example 14 (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 mixture was stirred at room temperature for 4 hours. Water (560 ml) was added dropwise to the reaction mixture, and the mixture was stirred for 30 minutes,-cooled on ice, and then stirred further for 1 hour. The crude crystal was recovered by a filtration, washed with water, dried in air, and then suspended in a 1:1 solvent mixture (250 ml) of ethyl acetate and diisopropylether, and the suspension was stirred at 25 to 40° C. for 1 hour, and then stirred with cooling on ice for 1 hour, and the crystal precipitated out was recovered by a filtration and washed with the solvent mixture described above (125 ml) to obtain the title compound (44.6 g, 91.7%).

1. stirringthe mixture was stirred for 30 minutes
2. stirringstirred further for 1 hour
3. filtrationThe crude crystal was recovered by a filtration
4. washwashed with water
5. customdried in air
6. stirringthe suspension was stirred at 25 to 40° C. for 1 hour
7. stirringstirred
8. temperaturewith cooling on ice for 1 hour
9. customthe crystal precipitated out
10. filtrationwas recovered by a filtration
11. washwashed with the solvent mixture