HRID46544
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperaturethe solution is refluxed for 6 hours
- customOn completion of the reaction
- customthe solvent is removed
- dissolutionthe residue dissolved in ethyl acetate
- washThe solution is washed with 10% hydrochloric acid
- dry with materialan aqueous solution of sodium bicarbonate and then dried
- concentrationThe product is concentrated
- customthe residue purified by a silica gel column