反应详情

First, 0.50 g of (4-chlorobenzyl)malononitrile was dissolved in 10 ml of N,N-dimethylformamide, to which 0.16 g of sodium hydride (60% in oil) was added under ice cooling. After the evolution of hydrogen gas ceased, while stirring under ice cooling, 0.48 ml of 2,3-dichloropropene was added dropwise, followed by stirring at room temperature for 5 hours. Then, 10% hydrochloric acid was added to the reaction mixture, which was extracted with diethyl ether. The organic layer was successively washed with 10% hydrochloric acid, a saturated aqueous sodium chloride solution, dried over anhydrous magnesium sulfate, and then concentrated under reduced pressure. The residue was subjected to silica gel column chromatography to give 0.19 g of 2-(4-chlorobenzyl)-2-(2-chloro-2-propenyl)malononitrile (the present compound (1)).

1. additionwas added under ice cooling
2. stirringby stirring at room temperature for 5 hours
3. extractionwas extracted with diethyl ether
4. washThe organic layer was successively washed with 10% hydrochloric acid
5. dry with materiala saturated aqueous sodium chloride solution, dried over anhydrous magnesium sulfate
6. concentrationconcentrated under reduced pressure