反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
In a 50 ml four-neck flask fitted with a thermometer, a reflux condenser and a stirrer were placed 2-(1-hydroxypentyl)cyclopentanone (20 g) synthesized in Reference Example 1, N-iodosuccinimide (0.1 g) and toluene (10 ml), and water was removed under refluxing, followed by 4 hours of the reaction at 150° C. The reaction mixture was washed with water and the layers were separated from each other. Further, the resulting organic layer was washed with saturated brine and separated. The organic layer was evaporated on a rotary evaporator under reduced pressure to recover toluene, whereby a crude product was obtained. The product was distilled using a Claisen distillation apparatus to obtain 15.3 g of 2-pentyl-2-cyclopentenone (boiling point: 104° C./930 Pa; GC purity: 98.4%).
WORKUP
后处理
- customIn a 50 ml four-neck flask fitted with a thermometer, a reflux condenser and a stirrer
- customwas removed
- temperatureunder refluxing
- customfollowed by 4 hours of the reaction at 150° C
- washThe reaction mixture was washed with water
- customthe layers were separated from each other
- washFurther, the resulting organic layer was washed with saturated brine
- customseparated
- customThe organic layer was evaporated on a rotary evaporator under reduced pressure
- customto recover toluene, whereby a crude product
- customwas obtained
- distillationThe product was distilled
- distillationa Claisen distillation apparatus