反应详情

温度

120 °C

11.2 5-Benzyloxy-2-bromo-pyridine (0.53 mmol), sodium-tert.-butyl at (1.4 eq.), tris-(dibenzylidene-acetone)-dipalladium (0.01 eq.), BINAP (0.01 eq.) and 1-methyl-1H-pyrazole-3-amine (1.2 eq.) are filled under nitrogen in a microwave reaction vessel. Degassed Toluene (50 eq.) is added. The reaction suspension is heated to 120° C. for 10 min. Ethyl acetate is added to the reaction suspension and filtrated over celite. The solvent of the filtrate is removed in vacuo. “A11” is obtained after column chromatography (heptan/ethyl acetate) as a colourless powder in a yield of 29%; HPLC (method C): 1.60 min); LC-MS (m Method A): 1.008 min, 281.15 (M+H+); 1H-NMR (DMSO-d6, 500 MHz): δ [ppm] 8.859 (s, 1H), 7.886 (d, 1H, J=2.5 Hz), 7.449-7.429 (m, 3H), 7.400-7.370 (m, 2H), 7.342-7.308 (m, 2H), 7.246 (d, 1H, J=9.0 Hz), 6.169 (d, 1H, J=2.5 Hz), 5.062 (s, 2H), 3.709 (s, 3H).

1. filtrationfiltrated over celite
2. customThe solvent of the filtrate is removed in vacuo
3. custom“A11” is obtained after column chromatography (heptan/ethyl acetate) as a colourless powder in a yield of 29%
4. custom1.60 min
5. custom1.008 min, 281.15 (M+H+)