反应详情

10 g of 1-(3-Chloro-5-trifluoromethyl-pyridin-2-yl)-cyclopropanecarbonitrile (step 1 of preparation example 1) was dissolved in 200 ml of methanol and 50 ml of ammonia (7N solution in methanol) was added, followed by 3 g of Raney Nickel. The reactor was sealed and the reaction mixture was stirred under 3 bar of hydrogen at ambient temperature for 2 hours. Then additional 5 g of Raney Nickel were added and the reaction mixture was stirred under 3 bar of hydrogen at ambient temperature for another 15 hours. Then the reaction mixture was filtered over celite and the filtrate was concentrated. Thus, 9.41 g of crude C-[1-(3-chloro-5-trifluoromethyl-pyridin-2-yl)-cyclopropyl]-methylamine was obtained as an orange oil, which was used for the next step without further purification. 1H-NMR (CDCl3): 8.72 ppm (s, 1H), 7.90 ppm (s, 1H), 3.00 ppm (s, 2H), 1.10 ppm (s, 2H, broad), 1.00 ppm (m, 2H), 0.90 ppm (m, 2H).

1. customThe reactor was sealed
2. filtrationThen the reaction mixture was filtered over celite
3. concentrationthe filtrate was concentrated