HRID568080
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
CONDITIONS
反应条件
- 温度
- 0 °C
PROCEDURE
实验过程
To a suspension of 140 g of nicotinic acid chloride hydrochloride in 500 ml of fluorobenzene cooled to 0° C. are added 280 g of aluminium chloride portionwise. The mixture is held under reflux for 6 hours, cooled and then poured onto ice. After the addition of sodium hydroxide up to pH=8, the mixture is extracted with dichloromethane. The organic phase is dried over magnesium sulphate and then evaporated under vacuum. The residue crystallises in a pentane/diisopropyl ether mixture giving 108.5 g of 3-(4-fluorobenzoyl)pyridine in the form of crystals melting at 91° C.
WORKUP
后处理
- temperatureunder reflux for 6 hours
- temperaturecooled
- additionpoured onto ice
- extractionthe mixture is extracted with dichloromethane
- dry with materialThe organic phase is dried over magnesium sulphate
- customevaporated under vacuum
- customThe residue crystallises in a pentane/diisopropyl ether mixture