反应详情

Benzoic acid (10 mg, 0.08 mmol) in DMF (0.2 mL) was treated with HATU (27 mg, 0.07 mmol) in DMF (0.2 mL) and DIPEA (30 μL, 0.24 mmol). The reaction mixture was shaken for five minutes prior to treatment with 6-(1H-indol-4-yl)-2-(tetrahydro-2H-pyran-2-yl)-2H-indazol-4-amine (20 mg, 0.06 mmol) in DMF (0.2 mL). Reaction mixture was shaken for five minutes and left to stand at 22° C. for 18 hrs. Solvent was removed in vacuo and the product re-dissolved in methanol (1 mL) prior to application on to an SCX cartridge (1 g). Product was eluted after 1 hr with 2M ammonia in methanol (2×3 mL), fractions were combined and concentrated under a stream of nitrogen using blow down apparatus. Purification by MDAP (Method D) afforded the title compound.

1. customReaction mixture
2. stirringwas shaken for five minutes
3. waitleft
4. waitto stand at 22° C. for 18 hrs
5. customSolvent was removed in vacuo
6. dissolutionthe product re-dissolved in methanol (1 mL)
7. washProduct was eluted after 1 hr with 2M ammonia in methanol (2×3 mL), fractions
8. concentrationconcentrated under a stream of nitrogen using blow down apparatus
9. customPurification by MDAP (Method D)