反应详情

温度

20 °C

2-Methyl-1,3-thiazole-4-carboxylic acid (4.59 g) (available from Maybridge), HATU (13.41 g) and DIPEA (16.80 ml) were stirred in DMF (140 ml) for 30 min at 20° C. 6-Bromo-1H-indazol-4-amine (3.4 g) (available from Sinova) was added and the reaction stirred at 20° C. for 2 days. The solvent was reduced to ˜40 ml and the reaction mixture was applied across 5×70 g aminopropyl SPE cartridges and left to stand for 3 h. The cartridges were eluted with DCM:methanol (1:1) and the combined solvent was evaporated in vacuo. The residue was suspended in DCM:methanol, adsorbed onto Florisil® and purified by chromatography on silica gel (100 g cartridge) eluting with 0-15% gradient of methanol (containing 1% triethylamine) in DCM over 60 min to give title compound (1.02 g).

1. waitleft
2. waitto stand for 3 h
3. washThe cartridges were eluted with DCM:methanol (1:1)
4. customthe combined solvent was evaporated in vacuo
5. custompurified by chromatography on silica gel (100 g cartridge)
6. washeluting with 0-15% gradient of methanol (containing 1% triethylamine) in DCM over 60 min