HRID1732436

反应详情

EQUATION

反应方程式

HRID 1732436 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
175 °C

PROCEDURE

实验过程

A 360 mg quantity of 5-methoxycarbonyl-4-methoxycarbonylmethyl-5-(cis-2-pentenyl)-2-cyclopentenone is dissolved in 8 ml of dimethyl sulfoxide containing 23 mg of water. The solution is reacted in a sealed tube with addition of 20 mg of sodium chloride. After the solution has been heated at 175° C. for 4 hours, the product is cooled to room temperature and then extracted with ethyl ether. The ethereal layer is washed, dried and distilled for the removal of the solvent. Purification of the residue by a silica gel column affords a compound (1-a) and compound (1-b) (R2 =CH3 in each). Yield of compound (1-a): 62.5%. Yield of compound (1-b): 28.5%. Combined yield: 91%. B.p. 87°-91° C./2.5 mm Hg.

WORKUP

后处理

  1. temperaturethe product is cooled to room temperature
  2. extractionextracted with ethyl ether
  3. washThe ethereal layer is washed
  4. customdried
  5. distillationdistilled for the removal of the solvent
  6. customPurification of the residue by a silica gel column