HRID2308072

反应详情

EQUATION

反应方程式

HRID 2308072 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

In a 100 ml four-neck flask fitted with a thermometer, a reflux condenser and a stirrer were placed 2-(1-hydroxyheptyl)cyclopentanone (40 g) synthesized in Reference Example 3, bromine (0.4 g) and n-octane (10 ml), and water was removed under refluxing, followed by 4 hours of the reaction at 120° C. The reaction mixture was washed with water and the layers were separated from each other. 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 n-octane, whereby a crude product (39 g) was obtained. The product was distilled using a Claisen distillation apparatus to obtain 32 g of 2-heptyl-2-cyclopentenone (boiling point: 111° C./900 Pa; GC purity: 97.8%).

WORKUP

后处理

  1. customIn a 100 ml four-neck flask fitted with a thermometer, a reflux condenser and a stirrer
  2. customwas removed
  3. temperatureunder refluxing
  4. customfollowed by 4 hours of the reaction at 120° C
  5. washThe reaction mixture was washed with water
  6. customthe layers were separated from each other
  7. washThe resulting organic layer was washed with saturated brine
  8. customseparated
  9. customThe organic layer was evaporated on a rotary evaporator under reduced pressure
  10. customto recover n-octane, whereby a crude product (39 g)
  11. customwas obtained
  12. distillationThe product was distilled
  13. distillationa Claisen distillation apparatus