反应详情

温度

0 °C

A solution of 4-azido-5-fluoropyridine-3-carbaldehyde (2.86 g, 17.2 mmol) and 2-amino-3-chlorobenzonitrile (2.62 g, 17.2 mmol) in DCM (60 mL) was cooled to 0° C. under an atmosphere of nitrogen. Triethylamine (7.2 mL, 51.6 mmol) was added, followed by dropwise additiona of titanium (IV) chloride solution (1 N in DCM, 10.3 mL, 10.3 mmol). The reaction mixture was stirred at 0° C. for 2 hours, then at room temperature overnight. The resultant mixture was concentrated under reduced pressure and the residue was dissolved in ethyl acetate and filtered through a pad of Celite®. The filtrate was concentrated under reduced pressure and the residue obtained was used in the following step without further purification.

1. customat room temperature
2. customovernight
3. concentrationThe resultant mixture was concentrated under reduced pressure
4. dissolutionthe residue was dissolved in ethyl acetate
5. filtrationfiltered through a pad of Celite®
6. concentrationThe filtrate was concentrated under reduced pressure
7. customthe residue obtained
8. customwas used in the following step without further purification