HRID46544

反应详情

EQUATION

反应方程式

HRID 46544 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

The compound (7) (500 mg) obtained above is dissolved in 200 ml of benzene containing 1 ml of acetic acid and 1 ml of piperidine, and the solution is refluxed for 6 hours. On completion of the reaction, the solvent is removed and the residue dissolved in ethyl acetate. The solution is washed with 10% hydrochloric acid and an aqueous solution of sodium bicarbonate and then dried. The product is concentrated, and the residue purified by a silica gel column, giving 5-methoxycarbonyl-4-methoxycarbonylmethyl-5-(2-pentynyl)-2-cyclopentenone (compound (2-a), R1 =R2 =CH3) in a yield of 81%, b.p. 110°-115° C./0.15 mm Hg.

WORKUP

后处理

  1. temperaturethe solution is refluxed for 6 hours
  2. customOn completion of the reaction
  3. customthe solvent is removed
  4. dissolutionthe residue dissolved in ethyl acetate
  5. washThe solution is washed with 10% hydrochloric acid
  6. dry with materialan aqueous solution of sodium bicarbonate and then dried
  7. concentrationThe product is concentrated
  8. customthe residue purified by a silica gel column