HRID277749

反应详情

EQUATION

反应方程式

HRID 277749 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1,1-Diethoxy-3-phenyl-3-cyclohexanecarbonyl-butane (74.4 g, 224 mmol) was dissolved in acetone (800 mL) followed by addition of 3.0 N HCl (800 mL). The reaction mixture was stirred for one hour at room temperature. It was then concentrated under vacuum to less than ½ its original volume and then extracted with methylene chloride (800 mL). The organic extract was then washed with brine (300 mL), dried over anhydrous magnesium sulfate, suction filtered and concentrated under vacuum to provide crude 3-phenyl-3-cyclohexanecarbonyl-butan-1-al (57.8 g). Alternatively, the dried and filtered methylene chloride solution can be used directly in the next step without concentration.

WORKUP

后处理

  1. concentrationIt was then concentrated under vacuum to less than ½ its original volume
  2. extractionextracted with methylene chloride (800 mL)
  3. extractionThe organic extract
  4. washwas then washed with brine (300 mL)
  5. dry with materialdried over anhydrous magnesium sulfate, suction
  6. filtrationfiltered
  7. concentrationconcentrated under vacuum