反应详情

First, 4.46 g of (3,4-dichlorobenzylidene)malononitrile was dissolved in 20 ml of tetrahydrofuran, and while stirring at room temperature, a suspension of 0.19 g of sodium borohydride in 5 ml of ethanol was added dropwise, followed by stirring at room temperature for 30 minutes. Then, 10% hydrochloride acid was added and the mixture 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 3.15 g of (3,4-dichlorobenzyl)malononitrile (the intermediate (12)).

1. additionwas added dropwise
2. stirringby stirring at room temperature for 30 minutes
3. extractionthe mixture was 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