HRID1153844
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
Morpholine (13.34 g), isovaleraldehyde (13.18 g), p-toluene sulfonic acid (0.2 g), and toluene (300 ml) were combined and heated at reflux using a Soxhlet extractor containing magnesium sulfate to remove any water produced. After three hours the Soxhlet extractor was replaced with a condenser, and ethyl 4,6-dimethyl-2-oxo-2H-pyran-5-carboxylate (30 g) was added. The reaction mixture was heated under reflux for approximately 64 hours. The solvent was evaporated, and the resultant oil was distilled at atmospheric pressure to give 11.1 g of crude product which was chromatographed to yield ethyl 2,6-dimethyl-3-(1-methylethyl)benzoate (2.8 g).
WORKUP
后处理
- temperatureheated
- temperatureat reflux
- customto remove any water
- customproduced
- temperatureThe reaction mixture was heated
- temperatureunder reflux for approximately 64 hours
- customThe solvent was evaporated
- distillationthe resultant oil was distilled at atmospheric pressure
- customto give 11.1 g of crude product which
- customwas chromatographed