反应详情

温度

70 °C

4-(2,3-diamino-5-chloropyridin-4-ylamino)-1,7,7-trimethylbicyclo[2.2.1]heptan-2-one (10) (380 mg, 1.23 mmol), 1-methyl-1H-pyrazole-4-carbaldehyde (135 mg, 1.23 mmol) were taken in EtOH (15 ml) to which ammonium acetate (112 mg) was added and the reaction mixture was heated at 70° C. for 48 h. Crude LCMS showed the desired product along with trace of starting material. The reaction mixture was allowed to come to rt and the precipitated was filtered and washed well with ethanol to afford the desired product (478 mg, 25%) as an off white solid. NMR: δ (1H, 400M Hz, DMSO-d6): 0.90 (3H, s), 0.91 (3H, s), 1.09 (3H, s), 1.40-1.80 (3H, m), 2.30-2.60 (1H, m), 3.00-3.10 (1H, m), 3.51-3.70 (1H, m), 3.93 (3H, s), 5.36 (1H, s), 8.00 (1H, s), 8.04 (1H, s), 8.31 (1H, s), 13.09 (1H, s). LCMS (254 nm): [M+H]+ 399.00 (96.43%). HPLC: 254 nm (94.06%)

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