反应详情

A mixture of 2-chloro-5-nitropyrimidin-4-amine (1.0 g, 5.8 mmol) and methylamine (2.0 M solution in THF, 14 mL, 28 mmol) was allowed to stir in a sealed vessel for 1 h. The mixture was then heated to 60 deg. C. for 30 min. The reaction was cooled to ambient temperature, and an additional amount of methylamine (2.0 M solution in THF, 8 mL, 16 mmol) was added and the reaction was sealed and heated to 60 deg. C. for 30 min. The reaction was cooled, diluted with water, and the precipitate was collected by filtration. The solid was rinsed with small portions of water followed by diethyl ether. The material was dried in under reduced pressure to give N2-methyl-5-nitropyrimidine-2,4-diamine 48 as a light yellow solid. MS (ES'): 170 (M+H)+; Calc. for C5H7N5O2=169.14.

1. temperatureThe mixture was then heated to 60 deg. C
2. waitfor 30 min
3. customthe reaction was sealed
4. temperatureheated to 60 deg. C
5. waitfor 30 min
6. temperatureThe reaction was cooled
7. filtrationthe precipitate was collected by filtration
8. washThe solid was rinsed with small portions of water
9. customThe material was dried in under reduced pressure