反应详情

温度

90 °C

6-(Chloromethyl)-N-[6-{6-chloro-5-[(methylsulfonyl)amino]-3-pyridinyl}-1-(phenylsulfonyl)-1H-indazol-4-yl]-2-pyridinecarboxamide (50 mg, 0.079 mmol) and piperidine (0.5 ml, 5.05 mmol) were placed in a vial and heated in a microwave at 90° C. for 15 min. The piperidine was blown off under a stream of nitrogen to give a yellow gum. The crude residue was suspended in IPA (2 ml) and 2M NaOH (1 ml) added. The mixture was stirred at room temperature for 2 hours. The solution was neutralised with 2M HCl (aq.) and then the solvent was blown off under a stream of nitrogen. The residue was dissolved in DMF/Acetone/Water (0.3 ml:0.3 ml:30 μl) (the insoluble salt was filtered off through a filter tube) and purified by MDAP (Method E). The solvent was evaporated under a stream of nitrogen to give a brown oil which was not completely clean, so further HPLC purification was carried out. The residue was dissolved in dioxane/water (1:1, 2 ml) and freeze dried to give the title compound as a white solid (3 mg).

1. customto give a yellow gum
2. filtrationwas filtered off through a filter tube) and
3. custompurified by MDAP (Method E)
4. customThe solvent was evaporated under a stream of nitrogen
5. customto give a brown oil which
6. customso further HPLC purification
7. dissolutionThe residue was dissolved in dioxane/water (1:1, 2 ml)
8. customfreeze dried