反应详情

温度

65 °C

1.2 g of Pd[P(Ph)3]4 and 7.6 g of p-fluorobenzeneboronic acid are added to a solution of 14.3 g of 5-bromonicotinic acid morpholinamide in 100 g of THF. A solution of 8.0 g of Na2CO3 in 25 g of water is subsequently added dropwise with stirring at 65° C. After 16 hours, the reaction mixture is cooled and evaporated in a rotary evaporator. The residue is taken up in dichloromethane, activated carbon is added, and the mixture is filtered. Repeated extraction of the filtrate with water and evaporation in a rotary evaporator gives a residue of 15.7 g, which, according to HPLC, comprises 89% of 5-(4-fluorophenyl)pyridine-3-carboxylic acid morpholinamide (net yield 93% of theory). Recrystallisation from ethyl acetate gives 8.0 g of 5-(4-fluorophenyl)pyridine-3-carboxylic acid morpholinamide having an HPLC purity of 99.6% (53.3% of theory).

1. temperaturethe reaction mixture is cooled
2. customevaporated in a rotary evaporator
3. additionactivated carbon is added
4. filtrationthe mixture is filtered
5. extractionextraction of the filtrate
6. customwith water and evaporation
7. customin a rotary evaporator
8. customgives a residue of 15.7 g, which