HRID2391044

反应详情

EQUATION

反应方程式

HRID 2391044 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1-(Biphenyl-4-yl)cyclopropanecarbonitrile (63 g, 288 mmol), KOH (1130 mmol) and ethylene glycol (350 mL) were heated to 160° C. for 6 hours (reaction complete by LCMS). The solution was cooled to room temperature, water (1.5 L) was added and the solution acidified to precipitate the product. The product was filtered overnight on a large Buchner (product formed a gel like suspension). The resulting wet solid was extracted with CH2Cl2 (˜2 L) and water, dried and evaporated to yield ˜60 g of 1-(biphenyl-4-yl)cyclopropanecarboxylic acid that was used as such in the next step.

WORKUP

后处理

  1. custom(reaction complete by LCMS)
  2. customto precipitate the product
  3. filtrationThe product was filtered overnight on a large Buchner (product
  4. customformed a gel like suspension)
  5. extractionThe resulting wet solid was extracted with CH2Cl2 (˜2 L) and water
  6. customdried
  7. customevaporated