反应详情

温度

50 °C

Added to a solution of 0.22 g (0.36 mmol) of 2-{4-[2-(4-fluorophenyl)-8-methyl-3-{1-[phenylsulphonyl]-1H-pyrrolo[2,3-b]pyridin-4-yl}imidazo[1,2-b]pyridazin-6-yl]piperazin-1-yl}ethanol in 5 ml of a mixture of tetrahydrofuran and methanol (1/1), is 0.12 ml (0.72 mmol) of a 6N aqueous solution of sodium hydroxide. The mixture is heated at 50° C. for 1 hour, then poured into 20 ml of water. The product is extracted with dichloromethane. The organic phase is separated, dried over sodium sulphate and the solvent is removed by evaporation under reduced pressure. The yellowish residue obtained is then purified by chromatography on a silica gel column (40 g) by eluting with a mixture of dichloromethane, methanol and aqueous ammonia (95/5/0.5) in order to give 0.110 g of 2-{4-[2-(4-fluorophenyl)-8-methyl-3-(1H-pyrrolo[2,3-b]pyridin-4-yl)imidazo[1,2-b]pyridazin-6-yl]piperazin-1-yl}ethanol after crystallization in 10 ml of acetonitrile, filtration and drying.

1. extractionThe product is extracted with dichloromethane
2. customThe organic phase is separated
3. dry with materialdried over sodium sulphate
4. customthe solvent is removed by evaporation under reduced pressure
5. customThe yellowish residue obtained
6. customis then purified by chromatography on a silica gel column (40 g)
7. washby eluting with a mixture of dichloromethane, methanol and aqueous ammonia (95/5/0.5) in order