反应详情

温度

-78 °C

2.0 g of 2,3-difluoro-6-trifluoromethylbenzonitrile was dissolved in 20 ml of anhydrous dichloromethane and the resultant solution was cooled down to -78° C. under a nitrogen atmosphere. To the solution was then gradually added dropwise with 7.1 ml of 1.5 M toluene solution of diisobutyl aluminium hydride (DIBAL) over 30 minutes. After stirring the solution at -78° C. for 1 hour, the solution was allowed to room temperature. The solution was then added with 7 ml of saturated aqueous solution of ammonium chloride, stirred for 30 minutes and subsequently added with 33 ml of 5% sulfuric acid. The mixture was then extracted with ether, and the organic layer obtained was washed with saturated saline solution and was then dried over anhydrous magnesium sulfate. After a process for the concentration, the organic solution was purified by using silica gel column chromatography to obtain 1.36 g of the title compound (nD 20.6-1.4357).

1. customwas allowed to room temperature
2. stirringstirred for 30 minutes
3. extractionThe mixture was then extracted with ether
4. customthe organic layer obtained
5. washwas washed with saturated saline solution
6. dry with materialwas then dried over anhydrous magnesium sulfate
7. concentrationAfter a process for the concentration
8. customthe organic solution was purified