HRID972103
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
A 790 mg quantity of the compound (3) obtained above is dissolved in 50 ml of benzene containing 1 ml of acetic acid and 1 ml of piperidine, and the solution is refluxed for 4 hours. On completion of the reaction, the solvent is removed, and the residue dissolved in ethyl acetate. The solution is washed with water and an aqueous solution of sodium bicarbonate and thereafter dried. The residue is distilled in a vacuum, giving 5-tert-butoxycarbonyl-4-methoxycarbonylmethyl-5-(2-pentynyl)-2-cyclopentenone (compound (1-a), R1 =t-Bu, R2 =CH3) in a yield of 78%, b.p. 82°-86° C./0.006 mm Hg.
WORKUP
后处理
- temperaturethe solution is refluxed for 4 hours
- customOn completion of the reaction
- customthe solvent is removed
- dissolutionthe residue dissolved in ethyl acetate
- washThe solution is washed with water
- dry with materialan aqueous solution of sodium bicarbonate and thereafter dried
- distillationThe residue is distilled in a vacuum