反应详情

温度

0 °C

A 250 ml three-necked flask equipped with a magnetic stirrer and an argon intake is charged with 4 g of 5-(2,6-difluorophenyl)-7-iodo-1H-pyrazolo[4,3-c]isoquinoline, prepared in step 6 of example 1, in 120 ml of THF and 3 ml of DMF. The mixture is cooled to 0° C. using an ice bath and then 952 mg of sodium hydride (60%) are added. After 15 min at 0° C., 1.3 ml of dimethylsulphamoyl chloride are added. After 16 h at RT, the mixture is poured into 300 ml of water and extracted with ethyl acetate. The organic phase is dried over MgSO4, filtered and concentrated under RP. The solid obtained is triturated in diisopropyl ether. The insoluble material is filtered off under RP and dried under vacuum to give 2.94 g of 5-(2,6-difluorophenyl)-7-iodo-N,N-dimethyl-1H-pyrazolo[4,3-c]isoquinoline-1-sulphonamide (beige solid). LC-MS-DAD-ELSD: 515(+)=(M+H)(+).

1. customA 250 ml three-necked flask equipped with a magnetic stirrer
2. waitAfter 16 h at RT
3. extractionextracted with ethyl acetate
4. dry with materialThe organic phase is dried over MgSO4
5. filtrationfiltered
6. concentrationconcentrated under RP
7. customThe solid obtained
8. customis triturated in diisopropyl ether
9. filtrationThe insoluble material is filtered off under RP
10. customdried under vacuum