反应详情

Under an argon atmosphere, 2.000 g (5.389 mmol) of the compound from example 24A were dissolved in 200 ml of 1,4-dioxane, and 9.378 g (16.167 mmol) of hexabutyldistannane were added. Added to the mixture were 2.000 g (1.731 mmol) of tetrakis(triphenylphosphine)palladium(0) and 0.910 g (5.928 mmol) of 2-chloro-7H-pyrrolo[2,3-d]pyrimidine (described in Bioorg. Med. Chem. 17(19), 6926-6936; 2009). The mixture was heated to reflux for 60 h. After cooling, the reaction mixture was filtered through Celite and the filtrate was concentrated on a rotary evaporator. The residue was stirred successively with ethyl acetate, acetonitrile and dimethyl sulfoxide. Subsequently, the residue was dissolved in trifluoroacetic acid, and acetonitrile and water were added until slight turbidity. The mixture was filtered and the filtrate was concentrated on a rotary evaporator and the residue was dried under high vacuum. 161 mg (8% of theory) of the title compound were obtained.

1. additionAdded to the mixture
2. temperatureThe mixture was heated
3. temperatureto reflux for 60 h
4. temperatureAfter cooling
5. filtrationthe reaction mixture was filtered through Celite
6. concentrationthe filtrate was concentrated on a rotary evaporator
7. dissolutionSubsequently, the residue was dissolved in trifluoroacetic acid
8. additionacetonitrile and water were added until slight turbidity
9. filtrationThe mixture was filtered
10. concentrationthe filtrate was concentrated on a rotary evaporator
11. customthe residue was dried under high vacuum