反应详情

温度

50 °C

The title compound was prepared from 3-(2-dimethylamino-6-methyl-pyrimidin-4-yl)-benzoic acid methyl ester [prepared by the following procedure: A mixture of NaH (50% dispersion in mineral oil, 1.56 g, 32.5 mmol) in 2-propanol (45 ml) was stirred at 50° C. for 10 min. N-methylguanidine hydrochloride (3.3 g, 30 mmol) was added and stirring was continued for 10 min. After the addition of 3-(3-oxo-butyryl)-benzoic acid (3.1 g, 15 mmol), the mixture was stirred at 80° C. for 48 h. After cooling to RT, H2O (100 ml) was added and the mixture was concentrated in vacuum to a volume of ca. 80 ml. The pH was set to 2.5 with 25% HCl and the precipitate was collected, dried and then esterified by stirring in 1N HCl-MeOH (30 ml) for 60 h at RT The crude product was purified by chromatography (silica gel, AcOEt) to give the methyl ester as light yellow solid (0.27 g).] (0.26 g, 1 mmol) by treatment with lithium tert-butyl acetate according to general procedure K (method b). Obtained as a light yellow oil (0.38 g, crude product).

1. customprepared by the following procedure
2. stirringstirring
3. waitwas continued for 10 min
4. stirringthe mixture was stirred at 80° C. for 48 h
5. temperatureAfter cooling to RT
6. concentrationthe mixture was concentrated in vacuum to a volume of ca. 80 ml
7. customthe precipitate was collected
8. customdried
9. stirringby stirring in 1N HCl-MeOH (30 ml) for 60 h at RT The crude product
10. customwas purified by chromatography (silica gel, AcOEt)