反应详情

温度

130 °C

2-Amino-6-chloro-N-(5-phenoxy-thiophen-2-ylmethyl)-nicotinamide described in Example A-101 (100 mg, 0.28 mmol) was dissolved in a mixture solution of dimethylsulfoxide (2 mL) and N,N-diisopropylethylamine (1 mL), 2-ethoxyethylamine (0.051 mL, 0.49 mmol) was added thereto, followed by heating in a sealed tube for 32 hours 40 minutes (oil bath temperature: 130° C.). The reaction mixture was allowed to room temperature, poured into brine, and the solution was extracted with ethyl acetate. The organic layer was dried over anhydrous magnesium sulfate, then concentrated, the obtained residue was purified by NH silica gel column chromatography (ethyl acetate:hexane=2:1), and the title compound (37 mg, 0.09 mmol, 32%) was obtained.

1. additionwas added
2. customwas allowed to room temperature
3. extractionthe solution was extracted with ethyl acetate
4. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
5. concentrationconcentrated
6. customthe obtained residue was purified by NH silica gel column chromatography (ethyl acetate:hexane=2:1)