反应详情

温度

65 °C

Sodium hydride (3.1 mg, 0.078 mmol, 60% in oil), catalytic amount of copper(I) iodide, 2-amino-6-chloro-N-(5-phenoxy-thiophen-2-ylmethyl)-nicotinamide described in Example A-102 (4.0 mg, 0.011 mmol) were added sequentially to ethyleneglycol (0.7 mL), and the solution was stirred at 65° C. for 2 hours. After further stirring at 90° C., the solution was allowed to cool to room temperature. Water, dichloromethane and an aqueous solution of saturated ammonium chloride were added to the reaction solution for extraction, which was then washed with brine, then, the solvent was evaporated in vacuo. The residue was purified by reverse phase high performance liquid chromatography (acetonitrile-water mobile phase (containing 0.1% trifluoroacetic acid) was used), and trifluoroacetic acid salt of the title compound (0.26 mg, 0.00052 mmol, 4.7%) was obtained.

1. stirringAfter further stirring at 90° C.
2. temperatureto cool to room temperature
3. washwas then washed with brine
4. customthe solvent was evaporated in vacuo