HRID359068

反应详情

EQUATION

反应方程式

HRID 359068 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

p-Methyl hydroxybenzoate (40 g) and potassium carbonate (54.5 g) in N,N-dimethylformaldehyde (200 ml) were heated with stirring at 100° C. for 1 hour, cooled to 40° C., and then, after adding 1-bromo-3-chloropropane (28.5 ml), the mixture was reacted at 60° C. for 2 hours. After cooling the reaction mixture, water and ethyl acetate were added thereto, and the mixture was separated into layers. The organic layer was washed with water 3 times, concentrated under reduced pressure. To the oily product thus obtained, a small amount of ethyl acetate and n-hexane were added. After the mixture was allowed to stand, the precipitated crystal was collected by filtration and the filtrate was again concentrated under reduced pressure to give the crystal of methy 4-(3-chloropropoxy)benzoate (56.92 g). mp. 52°-55° C.

WORKUP

后处理

  1. temperaturecooled to 40° C.
  2. customthe mixture was reacted at 60° C. for 2 hours
  3. additionwere added
  4. customthe mixture was separated into layers
  5. washThe organic layer was washed with water 3 times
  6. concentrationconcentrated under reduced pressure
  7. customTo the oily product thus obtained
  8. filtrationthe precipitated crystal was collected by filtration
  9. concentrationthe filtrate was again concentrated under reduced pressure