反应详情

[2-Chloro-6-(4-fluoro-phenyl)-pyrido[3,2-d]pyrimidin-4-yl]-(2,2,2-trifluoroethyl)-amine (100 mg, 0.28 mmol), 4-aminomethyl-N,N-dimethyl-benzamide (100 mg, 0.56 mmol) and diisopropylethylamine (0.097 mL, 0.56 mmol) were suspended in NMP (1.5 mL), sealed and heated by microwave to 140 deg C. for 1 h. After cooling the reaction mixture was added dropwise to a stirring mixture of water/acetonitrile (8 mL, 3:1) to afford a yellow precipitate. The solid was filtered, washed with water, dissolved in hot dioxane and concentrated onto silica gel. Purification by flash chromatography (0-10%, EtOH (containing 11% saturated aqueous ammonium hydroxide) in dichloromethane) to afford 21 mg (15%) of the desired product as a white solid. MS (m/z) 499.3 [M+H]+.

1. customsealed
2. temperatureheated by microwave to 140 deg C
3. temperatureAfter cooling the reaction mixture
4. customto afford a yellow precipitate
5. filtrationThe solid was filtered
6. washwashed with water
7. dissolutiondissolved in hot dioxane
8. concentrationconcentrated onto silica gel
9. customPurification by flash chromatography (0-10%, EtOH (containing 11% saturated aqueous ammonium hydroxide) in dichloromethane)