反应详情

A solution of 249 mg (0.97 mmol) of 2-(morpholin-4-yl)-3-trifluoromethyl-5-cyanopyridine (from Step D) in 5 mL 1:1 v/v 5 N NaOH/EtOH was heated at reflux for 1 h. The mixture was cooled and partitioned between 20 mL of ether and 20 mL of water. The aqueous layer was separated and adjusted to pH=4 with conc. HCl. The precipitated solid was filtered, rinsed with water and dried to afford 138 mg of the title compound: 1H NMR (500 MHz, CD3OD) δ 3.52 (app t, J=5.0, 4H), 3.78 (app t, J=5.0, 4H), 8.40 (d, J=2.0, 1H), 8.90 (d, J=2.0, 1H); ESI-MS (m/z) 277.3; HPLC A: 2.71 min.

1. temperatureat reflux for 1 h
2. temperatureThe mixture was cooled
3. custompartitioned between 20 mL of ether and 20 mL of water
4. customThe aqueous layer was separated
5. filtrationThe precipitated solid was filtered
6. washrinsed with water
7. customdried