反应详情

温度

-15 °C

3-(4,6-Dimethoxy-1,3,5-triazin-2-yl)-7-methoxy-1,3-dihydro-2H-indol-2-one (1.0 g) and 1-methyl-1H-imidazole (0.47 g) are introduced as initial charge in 8 ml of dichloromethane and cooled to −15° C. with nitrogen. With stirring, difluoromethanesulfonyl chloride (0.62 g) is added dropwise in two portions and the mixture is heated to 10° C. in 2.5 hours. It is cooled to 0° C., 1-methyl-1H-imidazole (0.24 g) and difluoromethanesulfonyl chloride (0.35 g) are added, and the mixture is warmed to room temperature over the course of 3 hours, after-stirred for 4 hours and left to stand for 48 hours. For work-up, water is added and the mixture is stirred, and the solid is filtered off, washed with dilute hydrochloric acid and water and dried. This gives the title compound as a solid in an HPLC purity of 91% (0.52 g, 39% of theory). The UV absorption (maximum at 360 nm) verifies the N-sulfonylation of the product.

1. temperaturethe mixture is heated to 10° C. in 2.5 hours
2. temperatureIt is cooled to 0° C.
3. temperaturethe mixture is warmed to room temperature over the course of 3 hours
4. stirringafter-stirred for 4 hours
5. waitleft
6. stirringthe mixture is stirred
7. filtrationthe solid is filtered off
8. washwashed with dilute hydrochloric acid and water
9. customdried