反应详情

温度

100 °C

A suspension of 4-(6-chloro-pyridazin-3-yl)-benzonitrile (1 g, 4.64 mmol; prepared as described in U.S. Pat. No. 4,112,095), isopropylpiperazine (0.654 g, 5.1 mmol), DIPEA (1.199 g, 9.27 mmol) and 4-(dimethylamino)pyridine (0.057 g, 0.464 mmol) in DMSO (4 ml) was stirred and heated to 100° C. for 20 h. After cooling to room temperature, the mixture was diluted with dichloromethane (25 ml) and water (35 ml) and stirred for 5 min. The organic phase was separated, washed with water (50 ml) and brine (50 ml), and acidified to pH 2 by addition of 1 N hydrochloric acid. The mixture was extracted with water (30 ml), and the aqueous phase was washed with dichloromethane (10 ml) and concentrated in vacuo to give a solid, which was collected and stripped with ethanol to afford the title compound as a crystalline hydrochloride (1.33 g, 76%).

1. customprepared
2. temperatureAfter cooling to room temperature
3. customThe organic phase was separated
4. washwashed with water (50 ml) and brine (50 ml)
5. additionacidified to pH 2 by addition of 1 N hydrochloric acid
6. extractionThe mixture was extracted with water (30 ml)
7. washthe aqueous phase was washed with dichloromethane (10 ml)
8. concentrationconcentrated in vacuo
9. customto give a solid, which
10. customwas collected