反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 70 °C
PROCEDURE
实验过程
7.1 g (53 mmol) of aluminum chloride are placed in 70 ml of nitrobenzene in a round-bottomed flask and under a stream of nitrogen. The mixture is heated at 70° C. until dilution is complete. It is then cooled to 0° C. and 7.2 ml (52 mmol) of 2-propylphenol are added. The mixture is allowed to warm to room temperature and is then heated to 40° C. 4.6 ml (52 mmol) of propionyl chloride are then added dropwise. The reaction medium is heated at 40° C. for 2 hours and then stirred for 48 hours at room temperature. It is then poured into ice with 20 ml of concentrated hydrochloric acid. After extraction with ethyl ether, the organic phase is washed with 2N sodium hydroxide. The aqueous phases are acidified with hydrochloric acid and extracted with ether. The organic phase is dried over magnesium sulfate, filtered and then evaporated. The black solid obtained is triturated in heptane, filtered off and dried. 3.5 g (35%) of the expected product are obtained in the form of a black powder.
WORKUP
后处理
- temperatureIt is then cooled to 0° C.
- temperatureto warm to room temperature
- temperatureis then heated to 40° C
- temperatureThe reaction medium is heated at 40° C. for 2 hours
- extractionAfter extraction with ethyl ether
- washthe organic phase is washed with 2N sodium hydroxide
- extractionextracted with ether
- dry with materialThe organic phase is dried over magnesium sulfate
- filtrationfiltered
- customevaporated
- customThe black solid obtained
- customis triturated in heptane
- filtrationfiltered off
- customdried