反应详情

温度

100 °C

A 50-mL round-bottomed flask equipped with a magnetic stirrer was charged with 4-chloro-2-{4,4-dimethyl-9-oxo-7-thia-10,11-diazatricyclo[6.4.0.02,6]dodeca-1(8),2(6),11-trien-10-yl}pyridine-3-carbaldehyde 282i (72 mg, 0.20 mmol), 288a (102 mg, 0.30 mmol), PdCl2(dppf) (16 mg, 0.020 mmol), K3PO4 (85 mg, 0.40 mmol), sodium acetate (33 mg, 0.40 mmol), acetonitrile (10 mL), and water (0.5 mL). After bubbling nitrogen into the mixture for 10 minutes, a reflux condenser was attached to the flask and the mixture was heated at 100° C. for 1 h. It was then cooled to room temperature and filtered. The filtrate was concentrated under reduced pressure to afford 288b, which was used in the next step without further purification. MS-ESI: [M+H]+ 529.3.

1. customA 50-mL round-bottomed flask equipped with a magnetic stirrer
2. customAfter bubbling nitrogen into the mixture for 10 minutes
3. customa reflux condenser was attached to the flask
4. temperatureIt was then cooled to room temperature
5. filtrationfiltered
6. concentrationThe filtrate was concentrated under reduced pressure