反应详情

To a suspension, stirred at 20° C., of 2 g (6.96 mmol) of 5-fluoro-1-[(3-fluorophenyl)methyl]-1H-indole-2-carboxylic acid, prepared in step 1.1, in 80 mL of dry toluene are added 5.08 mL (69.62 mmol) of thionyl chloride. The reaction mixture is stirred for 2 hours at reflux and then concentrated under reduced pressure. The resulting product is taken up in 10 mL of dichloromethane and this solution is poured, dropwise, into a solution of 9.12 mL (69.62 mmol) of 30% aqueous ammonia in water. The reaction mixture is stirred for 14 hours at 20° C. After this time, a solid is collected by filtration and triturated in 50 mL of diisopropyl ether. After filtering and drying under reduced pressure, 0.58 g of expected product is collected.

1. temperatureat reflux
2. concentrationconcentrated under reduced pressure
3. additionthis solution is poured
4. stirringThe reaction mixture is stirred for 14 hours at 20° C
5. filtrationAfter this time, a solid is collected by filtration
6. customtriturated in 50 mL of diisopropyl ether
7. filtrationAfter filtering
8. dry with materialdrying under reduced pressure, 0.58 g of expected product
9. customis collected