反应详情

温度

65 °C

Treat a solution of 3,3-dimethylbutan-1-amine (0.080 g, 0.790 mmol) and prop-1-en-2-yl (4-bromo-2-fluoro-5-(7-methyl-2-(methylthio)pyrido[2,3-d]pyrimidin-6-yl)phenyl)carbamate (0.244 g, 0.527 mmol) in dioxane (5 mL) with 1-methylpyrrolidine (4.48 mg, 0.053 mmol), heat at 65° C. for 3 h, then cool to RT overnight. Collect the resulting solid via filtration; concentrate the filtrate to dryness and purify via silica gel chromatography (10-30% EtOAc/DCM). Combine the two solids to afford the title compound (260 mg, 97% yield). MS (m/z): 506.1/508.1 (M+1).

1. temperaturecool to RT overnight
2. customCollect the resulting solid
3. filtrationvia filtration
4. concentrationconcentrate the filtrate to dryness
5. custompurify via silica gel chromatography (10-30% EtOAc/DCM)