反应详情

2.8 g (12 mmol) of 3-chloro-phenyl-guanidine nitrate and 0.5 g (12 mmol) of sodium hydroxide are added to a suspension of 2.0 g (11.7 mmol) of 3-dimethylamino-1-(4-pyridyl)-2-propen-1-one [described in EP-A-0 233 461] in 100 ml of isobutanol and the reaction mixture is boiled under reflux for 5 hours. After cooling, the reaction product is isolated by filtration, washed with water and chromatographed (tetrahydrofuran). After crystallisation (tetrahydrofuran/diethyl ether), N-(3-chloro-phenyl)-4-pyridyl-2-pyrimidineamine is obtained; m.p. 167°-168°, Rf =0.38 (methylene chloride:methanol=9:1).

1. temperatureunder reflux for 5 hours
2. temperatureAfter cooling
3. customthe reaction product is isolated by filtration
4. washwashed with water
5. customchromatographed (tetrahydrofuran)
6. customAfter crystallisation (tetrahydrofuran/diethyl ether)