反应详情

温度

100 °C

Under argon, 3.85 g (10.91 mmol) of the compound from example 24A were initially charged in dioxane (100 ml) and the reaction mixture was purged with argon. Subsequently, 8.27 ml (16.36 mmol) of hexabutylditin and 2.96 g (12.00 mmol) of ethyl 6-amino-2-chloro-5-nitropyrimidine-4-carboxylate (prepared according to J. Chem. Res. 1989, 2086-2097) were added. Thereafter, 3.83 g (5.45 mmol) of bis(triphenylphosphine)palladium(II) chloride were added and the reaction mixture was stirred at 100° C. overnight. Thereafter, the mixture was cooled to RT and filtered through Celite, and the residue was washed with methanol. The filtrate was concentrated, and the residue was extracted by stirring with ethyl acetate and filtered off. The filtrate was concentrated and the residue was purified by means of prep. HPLC (eluent: acetonitrile/water with 0.1% formic acid gradient). This gave 1.36 g (71% purity, 14% of theory) of crude product, which was converted without further purification.

1. customthe reaction mixture was purged with argon
2. temperatureThereafter, the mixture was cooled to RT
3. filtrationfiltered through Celite
4. washthe residue was washed with methanol
5. concentrationThe filtrate was concentrated
6. extractionthe residue was extracted
7. stirringby stirring with ethyl acetate
8. filtrationfiltered off
9. concentrationThe filtrate was concentrated
10. customthe residue was purified by means of prep
11. customThis gave 1.36 g (71% purity, 14% of theory) of crude product, which was converted without further purification