反应详情

5-(3-(Tetrahydro-2H-pyran-2-yloxy)-1-propynyl)-2-pyridinylamine (Preparation 6, 30 mg) and diethyl 2-(((4-chlorobenzyl)amino)carbonyl)malonate (Preparation 5, 50 mg) are dissolved in xylene and heated to reflux for 3 h. The solvent is evaporated and the residue is crystallized from ether/hexanes and dried to afford 20 mg of the a brown solid. Physical characteristics: MS (ESI+) m/z 470 (M+H)+. 1H NMR (CDCl3) δ9.80, 9.12, 7.80, 7.52, 7.32, 7.27, 4.86, 4.65, 4.51, 3.90, 3.5-3.6, 1.55-1.9.

1. temperatureheated
2. temperatureto reflux for 3 h
3. customThe solvent is evaporated
4. customthe residue is crystallized from ether/hexanes
5. customdried
6. customto afford 20 mg of the a brown solid