反应详情

温度

-13 °C

A mixture of ethyl 7-bromoimidazo[1,2-a]pyridine-3-carboxylate (0.54 g, 2.0 mmol) and 3-cyclopropyl-1-((6-methylpyridin-2-yl)methyl)-1H-indazol-4-amine (0.56 g, 2.0 mmol; prepared as in Example 65, steps A1-A3) in THF (10 mL) was cooled to −13° C. using an ice/water/MeOH bath. A solution of 1.0M lithium bis(trimethylsilyl)amide (4.4 mL, 4.4 mmol) was added over 5 minutes keeping the internal temperature below −10° C. The mixture was stirred at −10° C. for 10 minutes, warmed to ambient temperature and concentrated to give an oily residue. The residue was dissolved using IPA (10 mL) and treated with a 10% aqueous ammonium chloride solution (20 mL) to give a slurry which was stirred overnight. The slurry was filtered to collect the solid which was dried under vacuum to give the product (0.89 g). MS (ES+APCI) m/z=501.0 (M+H).

1. customthe internal temperature below −10° C
2. temperaturewarmed to ambient temperature
3. concentrationconcentrated
4. customto give an oily residue
5. dissolutionThe residue was dissolved
6. customto give a slurry which
7. stirringwas stirred overnight
8. filtrationThe slurry was filtered
9. customto collect the solid which
10. customwas dried under vacuum