反应详情

A reaction flask was cooled to 0° and charged with 20 ml of diethylene glycol dimethyl ether/water solution (1/1 by volume) and sodium cyanide (0.78 g, 0.016 mole). The resultant solution was stirred, and 3-phenoxybenzaldehyde (1.98 g, 0.01 mole) was added in 5 ml of diethylene glycol dimethyl ether. 3-(2,2-Dichloroethenyl)-2,2-dimethylcyclopropanecarbonyl chloride (2.73 g, 0.012 mole) was added dropwise to the stirred reaction mixture at 20° over a 10 minute period. Stirring was continued for 2 hours. The reaction mixture was then extracted three times with 15 ml portions of diethyl ether, once with 15 ml of water, once with a 2 N solution of aqueous sodium hydroxide, three times with water (15 ml), dried over magnesium sulfate, and concentrated under reduced pressure to afford α-cyano-3-phenoxybenzyl 3-(2,2-dichloroethenyl)-2,2-dimethylcyclopropanecarboxylate (4.35 g, 90% pure glpc).

1. temperatureA reaction flask was cooled to 0°
2. extractionThe reaction mixture was then extracted three times with 15 ml portions of diethyl ether
3. dry with materialonce with 15 ml of water, once with a 2 N solution of aqueous sodium hydroxide, three times with water (15 ml), dried over magnesium sulfate
4. concentrationconcentrated under reduced pressure