反应详情

A solution of 2,6-dichloronicotinoyl chloride (62.5 g), ethyl 3,3-dimethylaminoacrylate (58.8 g) and triethylamine (69 g) in toluene (600 mL) was stirred at 90° C. for 1 hour then cooled and concentrated. The concentrate was dissolved in dichloromethane (60 mL), diluted with diethyl ether, and filtered. The filtrate was concentrated, and the concentrate was crystallized from dichloromethane/diethyl ether/hexanes.

1. temperaturethen cooled
2. concentrationconcentrated
3. dissolutionThe concentrate was dissolved in dichloromethane (60 mL)
4. additiondiluted with diethyl ether
5. filtrationfiltered
6. concentrationThe filtrate was concentrated
7. customthe concentrate was crystallized from dichloromethane/diethyl ether/hexanes