反应详情

温度

60 °C

A mixture of 2,4-dichloro-6-methylpyrimidine (30.0 g, 184 mmol), 5-cyclopropyl-1H-pyrazol-3-ylamine (22.6 g, 184 mmol) and diisopropylethylamine (46 mL, 278 mmol) in 1-butanol (50 mL) was heated to 60° C. for 65 h. The reaction was cooled to room temperature and diluted with ethyl acetate. The mixture was washed with 2 N sodium hydroxide, water and brine, then dried over sodium sulfate and concentrated on a rotary evaporator. The residue was treated with a small amount of acetonitrile, sonicated and then triturated with ether until a solid was formed. The solid was collected by filtration to give the desired product (23.0 g, 50%) as a yellow solid.

1. temperatureThe reaction was cooled to room temperature
2. washThe mixture was washed with 2 N sodium hydroxide, water and brine
3. dry with materialdried over sodium sulfate
4. concentrationconcentrated on a rotary evaporator
5. additionThe residue was treated with a small amount of acetonitrile
6. customsonicated
7. customtriturated with ether until a solid
8. customwas formed
9. filtrationThe solid was collected by filtration