反应详情

温度

120 °C

65 mg of {4-[4-(5-Amino-pyridin-2-yl)-phenyl]-cyclohexyl}-acetic acid methyl ester and 0.3 Ml of 2-chlorobenzoxazole were dissolved in 1.5 Ml of t-BuOH/DME (1:1) in a 5 Ml microwave tube with a stirring bar. 0.1 Ml of 4N—HCl in dioxane was added and the reaction vessel was sealed and heated at 120° C. for 2 hours by microwave. The reaction was diluted with ethyl acetate and the resulting precipitates were filtered and washed with ethyl acetate. The filter cake was dried by air in the suction funnel and analyzed by 1H-NMR (400 MHz, DMSO-d6) δ ppm 1.2 (s, 3H) 1.5 (s, 2H) 1.8 (s, 6H) 2.3 (d, J=6.8 Hz, 2H) 3.6 (s, 4H) 7.2 (m, 1H) 7.3 (m, 1H) 7.3 (d, J=8.3 Hz, 2H) 7.5 (d, J=13.9 Hz, 2H) 8.0 (m, 3H) 8.4 (m, 1H) 8.9 (d, J=2.3 Hz, 1H) 11.0 (s, 1H); (M+H)+442.2.

1. customthe reaction vessel was sealed
2. customthe resulting precipitates
3. filtrationwere filtered
4. washwashed with ethyl acetate
5. customThe filter cake was dried by air in the suction funnel