Bromine → HCID 10219687, compound

In a 100 ml four-neck flask fitted with a thermometer, a reflux condenser and a stirrer were placed 2-heptylidenecyclopentanone (20 g) synthesized in Reference Example 6, bromine (0.05 g) and tetrachloroethylene (10 ml), followed by 4 hours of the reaction under refluxing. 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 tetrachloroethylene, whereby a crude product (19 g) was obtained. The product was distilled using a Claisen distillation apparatus to obtain 16.8 g of 2-heptyl-2-cyclopentenone (boiling point: 111° C./900 Pa; GC purity: 97.3%).

1. customIn a 100 ml four-neck flask fitted with a thermometer, a reflux condenser and a stirrer
2. customfollowed by 4 hours of the reaction
3. temperatureunder refluxing
4. washThe reaction mixture was washed with water
5. customthe layers were separated from each other
6. washFurther, the resulting organic layer was washed with saturated brine
7. customseparated
8. customThe organic layer was evaporated on a rotary evaporator under reduced pressure
9. customto recover tetrachloroethylene, whereby a crude product (19 g)
10. customwas obtained
11. distillationThe product was distilled
12. distillationa Claisen distillation apparatus

ORD record

ord-95d30a89d2d84491b0315728b90b6570

Source dataset

uspto-grants-2004_12

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06833481B2