HRID463379
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
PROCEDURE
实验过程
A solution of ethyl 2-methoxyimino-3-oxobutyrate (syn isomer 17.3 g), ethylene glycol (12.4 g) and p-toluenesulfonic acid (0.5 g) in benzene (260 ml) was heated under reflux while removing water. The resultant solution was washed with a saturated aqueous solution of sodium bicarbonate and a saturated aqueous solution of sodium chloride in turn and dried over magnesium sulfate. After evaporating the solvent from the solution, the residue was distilled under reduced pressure to give ethyl 2-methoxyimino-3,3-ethylenedioxybutyrate (syn isomer, 15.2 g), bp 97° to 102° C./4 mmHg.
WORKUP
后处理
- temperatureunder reflux
- customwhile removing water
- washThe resultant solution was washed with a saturated aqueous solution of sodium bicarbonate
- dry with materiala saturated aqueous solution of sodium chloride in turn and dried over magnesium sulfate
- customAfter evaporating the solvent from the solution
- distillationthe residue was distilled under reduced pressure