反应详情

567 mg (1.13 mmol) of N-{4-[(3-chloro 1-{[2-(trimethylsilyl)ethoxy]methyl}-1H-pyrrolo[2,3-b]pyridin-4-yl)methyl]-3-fluorophenyl}-2,2,2-trifluoroacetamide are dissolved in 5 ml of dichloromethane. 5 ml (65 mmol) of trifluoroacetic acid are added, and the mixture is stirred at RT for 3 h. The mixture is then concentrated, EA is added and the mixture is washed with sat. sodium carbonate solution. The organic phase is dried over sodium sulfate and concentrated. The residue is taken up in 35 ml of THF, and 15 ml of water and 542 mg (22.7 mmol) of lithium hydroxide are added. The mixture is stirred at RT for 20 h. The mixture is then concentrated under reduced pressure, and the residue is diluted with water. The mixture is extracted with ethyl acetate and the extract is dried over sodium sulfate and concentrated. The residue is purified by chromatography on silica gel (mobile phase dichloromethane:methanol 25:1). This gives crystals.

1. concentrationThe mixture is then concentrated
2. additionEA is added
3. washthe mixture is washed with sat. sodium carbonate solution
4. dry with materialThe organic phase is dried over sodium sulfate
5. concentrationconcentrated
6. stirringThe mixture is stirred at RT for 20 h
7. concentrationThe mixture is then concentrated under reduced pressure
8. additionthe residue is diluted with water
9. extractionThe mixture is extracted with ethyl acetate
10. dry with materialthe extract is dried over sodium sulfate
11. concentrationconcentrated
12. customThe residue is purified by chromatography on silica gel (mobile phase dichloromethane:methanol 25:1)