反应详情

1-Ethyl-3-methyl-1H-pyrazole-5-carboxylic acid (67.8 mg) was treated with N-[(dimethylamino)(3H-[1,2,3]triazolo[4,5-b]pyridin-3-yloxy)methylidene]-N-methylmethanaminium hexafluorophosphate (168 mg) in DMF (750 μl) and DIPEA (150 μl). Reaction mixture was shaken for five min prior to treatment with 6-(1H-indol-4-yl)-1H-indazol-4-amine (50 mg) in DMF (350 μl). Reaction mixture was left to stand at 22° C. for 16 hrs. Solvent was removed in vacuo and the product re-dissolved in chloroform (0.3 ml) prior to application on to a preconditioned (methanol then chloroform) aminopropyl SPE cartridge (1 g). Product was eluted after 2 h with ethyl acetate:methanol (1:1, 3.2 ml), and concentrated under a stream of nitrogen using blow down apparatus. Purification by mass directed preparative HPLC (Method B) gave the title compound.

1. customReaction mixture
2. customReaction mixture
3. waitwas left
4. waitto stand at 22° C. for 16 hrs
5. customSolvent was removed in vacuo
6. dissolutionthe product re-dissolved in chloroform (0.3 ml)
7. washProduct was eluted after 2 h with ethyl acetate:methanol (1:1, 3.2 ml)
8. concentrationconcentrated under a stream of nitrogen using blow down apparatus
9. customPurification by mass