反应详情

To a solution of 1-(2-aminopyrimidin-4-yl)-6-bromoindazole-3-carboxylic acid (500 mg, 1.32 mmol) in DCM (5 mL), was added thionyl chloride (0.6 mL, 7.9 mmol) followed by DMF (0.02 mL). The mixture was stirred at RT for 1 hr. The mixture was concentrated in vacuo, DCM (2 mL) added and concentration in vacuo was repeated. To this residue was added THF (5 mL) and conc. aq NH3 (0.5 mL). The mixture stirred for 30 min, then diluted with water and the resultant solid was collected by suction filtration. The solid was thoroughly dried under high vacuum, to give the title compound (360 mg): 1H NMR (250 MHz, DMSO) delta 7.15 (1H, br. s.), 7.32 (1H, d, J=5.48 Hz), 7.60 (1H, dd, J=8.60, 1.60 Hz), 7.74 (1H, br. s.), 8.20 (1H, d, J=8.38 Hz), 8.38 (1H, d, J=5.48 Hz), 9.18 (1H, d, J=1.22 Hz); LC-MS: m/z=+332.90/334.70 (M+H)+.

1. concentrationThe mixture was concentrated in vacuo, DCM (2 mL)
2. additionadded
3. concentrationconcentration in vacuo
4. additionTo this residue was added THF (5 mL) and conc. aq NH3 (0.5 mL)
5. stirringThe mixture stirred for 30 min
6. additiondiluted with water
7. filtrationthe resultant solid was collected by suction filtration
8. customThe solid was thoroughly dried under high vacuum