HRID1972006

反应详情

EQUATION

反应方程式

HRID 1972006 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

3-Bromo-4-hydroxy-benzaldehyde (24.8 mmol, 5.0 g), bromo-cyclohexane (37.3 mmol, 6.08 g) and K2CO3 (37.3 mmol, 5.15 g) were suspended in DMF (15 mL) and stirred over night at 90° C. The mixture was cooled to room temperature, and bromo-cyclohexane (36.8 mmol, 6.0 g) and K2CO3 (36.2 mmol, 5.0 g) were added stirred at 90° C. for another 24 h. The mixture was cooled and filtered. The filtrate was extracted with ethyl acetate. The organic layer was washed with 1.0 N NaOH (200 mL), water, and brine, dried (Na2SO4), filtered, and concentrated under reduced pressure to provide 3-bromo-4-cyclohexyloxy-benzaldehyde (2.7 g).

WORKUP

后处理

  1. temperatureThe mixture was cooled to room temperature
  2. stirringstirred at 90° C. for another 24 h
  3. temperatureThe mixture was cooled
  4. filtrationfiltered
  5. extractionThe filtrate was extracted with ethyl acetate
  6. washThe organic layer was washed with 1.0 N NaOH (200 mL), water, and brine
  7. dry with materialdried (Na2SO4)
  8. filtrationfiltered
  9. concentrationconcentrated under reduced pressure