HRID1005392

反应详情

EQUATION

反应方程式

HRID 1005392 的结构方程式

PROCEDURE

实验过程

To a solution of 1-(4-iodophenyl)cyclopropane-1-carboxylic acid (7.98 g, 27 mmol) in methylene chloride (200 mL) containing DMF (0.25 mL) was added dropwise over 30 minutes oxalyl chloride (3.2 mL). The mixture was stirred for 1 hour, and the solvent was removed under reduced pressure. The residue was taken up in THF (100 mL), and potassium t butoxide (1 M in THF, 35 mL) was added. After 30 minutes, the mixture was diluted with hexane, washed with water, dried, filtered and evaporated. The solid residue was recrystallized from methanol to give t butyl 1-(4-iodophenyl)cyclopropane-1-carboxylate (5.74 g, 16.6 mmol, 62%).

WORKUP

后处理

  1. customthe solvent was removed under reduced pressure
  2. additionpotassium t butoxide (1 M in THF, 35 mL) was added
  3. waitAfter 30 minutes
  4. additionthe mixture was diluted with hexane
  5. washwashed with water
  6. customdried
  7. filtrationfiltered
  8. customevaporated
  9. customThe solid residue was recrystallized from methanol