反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 50 °C
PROCEDURE
实验过程
98 ml of glacial acetic acid were added dropwise, at 25° C., to 350 g of 3,5-dimethylpyridine. The mixture was heated to 50° C. and 870.3 g of 40% peracetic acid were metered in such that the temperature could be kept at 50° C. by cooling. About 1 hour after the addition of the peracetic acid had ended, the reaction mixture was cooled to 25° C. and 230 g of Na2SO3 in 1 1 of water were added dropwise, with cooling. After the excess peracetic acid had been destroyed (KI-starch test), 1330 ml of water were added, the mixture was rendered alkaline with 730 ml of 50% NaOH and the solution was extracted in several portions with a total of about 4500 ml of chloroform. The combined organic phases were dried with Na2SO4 and the solvent was evaporated off to about 740 ml.
WORKUP
后处理
- customcould be kept at 50° C.
- temperatureby cooling
- temperaturethe reaction mixture was cooled to 25° C.
- temperaturewith cooling
- customAfter the excess peracetic acid had been destroyed (KI-starch test), 1330 ml of water
- additionwere added
- extractionthe solution was extracted in several portions with a total of about 4500 ml of chloroform
- dry with materialThe combined organic phases were dried with Na2SO4
- customthe solvent was evaporated off to about 740 ml