HRID1657492

反应详情

EQUATION

反应方程式

HRID 1657492 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

0.684 g. Magnesium metal is covered with 2 ml. anhydrous tetrahydrofuran and 0.2 ml. 1,2-dibromoethane is added with stirring and heating. 1-Bromo-6-cyclopropylhexane (4.8 g.) and tetrahydrofuran (25 ml.) are added portionwise. An additional 0.207 ml. of 1,2-dibromoethane is added and the reaction mixture refluxed for 3 hours. The solution is then maintained at 24°-28° while anhydrous carbon dioxide is bubbled through it for 11/2 hours. After stirring overnight under carbon dioxide, dry ether, water and 2N sulfuric acid are added until the pH is less than 7. The solution is extracted with ether and washed with water and brine, dried over calcium sulfate, filtered and the solvent removed to yield 7-cyclopropylheptanoic acid.

WORKUP

后处理

  1. temperatureheating
  2. temperaturethe reaction mixture refluxed for 3 hours
  3. customis bubbled through it for 11/2 hours
  4. stirringAfter stirring overnight under carbon dioxide
  5. additiondry ether, water and 2N sulfuric acid are added until the pH is less than 7
  6. extractionThe solution is extracted with ether
  7. washwashed with water and brine
  8. dry with materialdried over calcium sulfate
  9. filtrationfiltered
  10. customthe solvent removed