反应详情

温度

20 °C

To 3-Methyl-2-pyridinecarboxylic acid (0.032 g, 0.234 mmol) in DMF (0.5 ml) was added HATU (0.089 g, 0.234 mmol) and the solution stirred for 10 min at 20° C. To this was then added a solution of 3-fluoro-6-(1H-indol-4-yl)-1H-indazol-4-amine (0.052 g, 0.195 mmol) in DMF (0.5 ml), followed by DIPEA (0.068 ml, 0.391 mmol) and the top was placed on the vial which had been pierced with a needle. The mixture was stirred at 20° C. for 66 hours then loaded directly onto a dry 1 g NH2 cartridge, left for 2 hours then eluted with methanol (2.5 column vols). Upon standing for 20 hours at 20° C., a solid precipitated from the orange solution which was filtered off and dried. The solid was triturated with methanol (2×2 ml) then blown to dryness and loaded onto a 500 mg SCX pre-rinsed with methanol. Elution with methanol (3 column vols) then 2M NH3/MeOH (3 column vols) and concentration of the basic fractions by blow down afforded the title compound (6 mg).

1. stirringThe mixture was stirred at 20° C. for 66 hours
2. waitleft for 2 hours
3. washthen eluted with methanol (2.5 column vols)
4. waitUpon standing for 20 hours at 20° C.
5. customa solid precipitated from the orange solution which
6. filtrationwas filtered off
7. customdried
8. customThe solid was triturated with methanol (2×2 ml)
9. washpre-rinsed with methanol
10. washElution with methanol (3 column vols)