反应详情

Treat a solution of 6-(5-amino-4-fluoro-2-methylphenyl)-N-(2-methoxyethyl)-7-methylpyrido[2,3-d]pyrimidin-2-amine (0.270 g, 0.791 mmol) in dioxane (5 mL) with 3,3-dimethylcyclobutane carboxylic acid (0.122 g, 0.949 mmol) followed by DPPA (0.261 g, 0.949 mmol) and TEA (0.160 g, 1.582 mmol), stir at RT for 20 minutes, heat to 90° C. for 2 h and then cool to RT overnight. Concentrate the mixture to dryness, purify via silica gel chromatography (20-100% EtOAc/Hexanes) and triturate with MeCN. Collect the resulting material via filtration and re-purify via silica gel chromatography (20-100% EtOAc/Hexanes) to afford the title compound as a yellow solid (55 mg, 13% yield). MS (m/z): 467.3 (M+1).

1. temperatureheat to 90° C. for 2 h
2. temperaturecool to RT overnight
3. concentrationConcentrate the mixture to dryness
4. custompurify via silica gel chromatography (20-100% EtOAc/Hexanes)
5. customtriturate with MeCN
6. customCollect the resulting material
7. filtrationvia filtration
8. customre-purify via silica gel chromatography (20-100% EtOAc/Hexanes)