HRID1905352

反应详情

EQUATION

反应方程式

HRID 1905352 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
200 °C

PROCEDURE

实验过程

A mixture of 70 g (0.61 mol) of trans-4-methyl-2-pentenoic acid and 49 g (0.72 mol) of 1,3-pentadiene was heated for 12 hours at approx. 200° C. in an autoclave. After the reaction mixture had cooled, it was checked by means of GLC for the presence of 4-methyl-2-pentenoic acid. A further 25 g (0.36 mol) of 1,3-pentadiene were added, after which the mixture was again heated for 12 hours at 200° C. This procedure was repeated until no further decrease in the content of 4-methyl-2-pentenoic acid was any longer observed. The reaction mixture obtained was dissolved in 300 ml of ether and extracted with 300 ml of 10% NaOH solution. The alkaline solution thus obtained was acidified with 40 g of concentrated sulphuric acid and then extracted three times with ether. The ether extract was washed with water, dried on MgSO4, evaporated down and distilled. 73 g of 6-isopropyl-2-methyl-3-cyclohexene-1-carboxylic acid were obtained, b.p.: 95°-100° C./70 Pa.

WORKUP

后处理

  1. temperatureAfter the reaction mixture had cooled
  2. temperatureafter which the mixture was again heated for 12 hours at 200° C
  3. customThe reaction mixture obtained
  4. extractionextracted with 300 ml of 10% NaOH solution
  5. customThe alkaline solution thus obtained
  6. extractionextracted three times with ether
  7. extractionThe ether extract
  8. washwas washed with water
  9. customdried on MgSO4
  10. customevaporated down
  11. distillationdistilled