反应详情

A suspension, stirred at 20° C., of 2 g (6.96 mmol) of 5-fluoro-1-(3-fluorobenzyl)-1H-indole-2-carboxylic acid, prepared according to the protocol described in step 1.1, in 80 ml of dry toluene is admixed with 5.08 ml (69.62 mmol) of thionyl chloride. The reaction mixture is stirred at reflux for 2 hours 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. The reaction mixture is stirred at 20° C. for 14 hours. After this time a solid is recovered by filtration and triturated in 50 ml of diisopropyl ether. Filtration and drying under reduced pressure give 0.58 g of expected product.

1. customprepared
2. temperatureat reflux for 2 hours
3. concentrationconcentrated under reduced pressure
4. stirringThe reaction mixture is stirred at 20° C. for 14 hours
5. filtrationAfter this time a solid is recovered by filtration
6. customtriturated in 50 ml of diisopropyl ether
7. filtrationFiltration
8. customdrying under reduced pressure