HRID568080

反应详情

EQUATION

反应方程式

HRID 568080 的结构方程式

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

  1. temperatureunder reflux for 6 hours
  2. temperaturecooled
  3. additionpoured onto ice
  4. extractionthe mixture is extracted with dichloromethane
  5. dry with materialThe organic phase is dried over magnesium sulphate
  6. customevaporated under vacuum
  7. customThe residue crystallises in a pentane/diisopropyl ether mixture