反应详情

温度

40 °C

3-Bromo-4-chloro-1-methyl-1H-pyrazolo[3,4-d]pyrimidin-6-ylamine (Intermediate 14) (160 mg, 0.61 mmol), benzylamine (0.2 ml, 1.83 mmol) and DMF (5 ml) are mixed together and heated at 40° C. overnight. After cooling to room temperature the solvent is removed in vacuo and the residue is dissolved in methanol (30 ml) and passed through an Isolute™ CBA column (silica based carboxylic acid sorbent). Silica gel is added to the filtrate, the solvent is removed in vacuo and the resulting residue is flash chromatographed eluting with EtOAc:iso-hexanes (4:6) and then increasing to EtOAc:iso-hexanes (1:1). The appropriate fractions are collected and concentrated in vacuo to afford the title compound.

1. temperatureAfter cooling to room temperature the solvent
2. customis removed in vacuo
3. dissolutionthe residue is dissolved in methanol (30 ml)
4. additionSilica gel is added to the filtrate
5. customthe solvent is removed in vacuo
6. customchromatographed
7. washeluting with EtOAc:iso-hexanes (4:6)
8. temperatureincreasing to EtOAc:iso-hexanes (1:1)
9. customThe appropriate fractions are collected
10. concentrationconcentrated in vacuo