反应详情

Into a 500 ml round bottom flask equipped with a thermometer, a dropping funnel and a Teflon blade stirrer were added a solution of 50 weight percent sodium hydroxide (41.9 grams, 0.52 mole) and 84 grams of distilled water. The solution was cooled to 15° C. by an ice bath and 50% hydrogen peroxide (18.4 grams, 0.27 mole) was added slowly through the dropping funnel. A sodium peroxide slurry formed immediately. The sodium peroxide slurry was transferred slowly into a 500 ml four-necked round bottom reactor flask containing 82.1 grams (0.5 mole) of the 1-cyano-1-methylethyl chloroformate of Example 1. The reactor flask was equipped with a Teflon blade stirrer, a bottom stopcock, a vent, a sodium peroxide slurry inlet and a thermometer. The temperature within the reactor flask was maintained at about 15° C. or less by spraying ice water on the outside of the flask. On completing the addition of the sodium peroxide slurry, 50 ml of distilled water was added to the reactor flask with stirring and a solid material precipitated immediately. The stirring was continued for 90 minutes. Thereafter, the solid precipitate (43.5 grams, 63% yield) was recovered by filtration, washed twice with distilled water and once with 2-propanol. The product was a white solid having a melting point of 58°-59° C. Identification of the product as di(1-cyano-1-methylethyl)peroxydicarbonate was confirmed by infrared and NMR spectroscopy. Iodometric titration of the product gave a percarbonate assay of 93%.

1. customThe reactor flask was equipped with a Teflon blade stirrer
2. temperatureThe temperature within the reactor flask was maintained at about 15° C. or less
3. additionwas added to the reactor flask
4. customa solid material precipitated immediately