反应详情

温度

120 °C

To a mixture of 3-(4-bromo-pyrazol-1-yl)-pyridin-2-ylamine (34 mg, 0.14 mmol) described in Manufacturing Example 39-1-4, (4-benzyloxy-benzyl)-tributyl-stannane (84 mg, 0.17 mmol) described in Manufacturing Example 39-2-1 and N-methylpyrrolidinone (1.5 mL) were added tri-o-tolylphosphine (17 mg, 0.057 mmol) and palladium (II) acetate (3.2 mg, 0.014 mmol) at room temperature, which was stirred for 5 hours at 120° C. The reaction mixture was cooled to room temperature, and filtered after addition of an aqueous potassium fluoride solution and ethyl acetate. The organic layer was separated, washed with saturated aqueous sodium chloride, and the solvent was evaporated under a reduced pressure. The residue was purified by reverse-phase high performance liquid chromatography (using an acetonitrile-water mobile phase containing 0.1% trifluoroacetic acid) to obtain the title compound (2.6 mg, 4%) as a trifluoroacetic acid salt.

1. temperatureThe reaction mixture was cooled to room temperature
2. filtrationfiltered
3. additionafter addition of an aqueous potassium fluoride solution and ethyl acetate
4. customThe organic layer was separated
5. washwashed with saturated aqueous sodium chloride
6. customthe solvent was evaporated under a reduced pressure
7. customThe residue was purified by reverse-phase high performance liquid chromatography (
8. additioncontaining 0.1% trifluoroacetic acid)