反应详情

0.20 g (0.84 mmol) of 5-chloro-2-(methylsulfonyl)pyrimidine-4-carboxylic acid, 0.15 g (1.01 mmol) of (1R)-1,2,3,4-tetrahydronaphthalene-1-amine and 0.33 g (1.69 mmol) of dicyclohexylmethylamine in 1.5 ml of N-methylpyrrolidone are heated in a closed cuvette in the microwave at 150° C. for 30 minutes (Biotage Initiator, http://www.biotage.com/DynPage.aspx?id=22001). The crude mixture obtained in this manner is applied to silica gel and purified by column chromatography using the mobile phase heptane/ethyl acetate. Concentration gives initially 0.024 g of 5-chloro-N-[(1R)-1,2,3,4-tetrahydronaphthalen-1-yl]pyrimidine-2-amine (solid) and then 0.08 g of 2-(methylsulfonyl)-N-[(1R)-1,2,3,4-tetrahydronaphthalen-1-yl]pyrimidine-5-amine (wax-like, yield 31% at a purity of 95%).

1. customThe crude mixture obtained in this manner
2. custompurified by column chromatography
3. concentrationConcentration