反应详情

温度

120 °C

2-Amino-6-chloro-N-(5-phenoxy-thiophen-2-ylmethyl)-nicotinamide (150 mg, 0.417 mmol) described in Preparation Example A+-11, ethane-1,2-diamine (418 μl, 6.25 mmol) were dissolved in a mixture solution of dimethylsulfoxide (2 mL) and N,N-diisopropylethylamine (1 mL), and the solution was stirred at 120° C. for 15 hours. The reaction solution was cooled to room temperature, water was added, then extracted with ethyl acetate and tetrahydrofuran, the organic layer was washed with brine and dried over anhydrous magnesium sulfate. The solvent was evaporated in vacuo, tetrahydrofuran and NH silica gel were added to the residue, the solvent was evaporated in vacuo adsorption, purification was carried out by NH silica gel column chromatography (ethyl acetate:methanol=10:1), and the title compound (95 mg, 0.25 mmol, 59%) was obtained as a white solid.

1. temperatureThe reaction solution was cooled to room temperature
2. extractionextracted with ethyl acetate and tetrahydrofuran
3. washthe organic layer was washed with brine
4. dry with materialdried over anhydrous magnesium sulfate
5. customThe solvent was evaporated in vacuo, tetrahydrofuran and NH silica gel
6. additionwere added to the residue
7. customthe solvent was evaporated in vacuo adsorption, purification