HRID1780847

反应详情

EQUATION

反应方程式

HRID 1780847 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

4-(3-Cyclopentyloxy-4-methoxyphenyl)-4-formylcyclohexan-1-one dimethyl ketal (0.1 g, 0.28 mmol) in ethyl acetate (2 mL) was treated with 3N hydrochloric acid (5 mL) and the mixture was stirred vigorously and gently heated for 10 min. The mixture was extracted twice with ethyl acetate, the combined organic extracts were washed with 5% aqueous sodium carbonate, dried (potassium carbonate) and the solvent was removed in vacuo. This material, combined with that obtained from an identical reaction, was purified by flash chromatography, eluting with 2% ethyl acetate/chloroform, to provide a white solid (0.1 g, 57%): m.p. 55°-57° C. Analysis Calc. for C19H24O4 : C 72.13, H 7.65; found: C 72.09, H 7.57.

WORKUP

后处理

  1. temperaturegently heated for 10 min
  2. extractionThe mixture was extracted twice with ethyl acetate
  3. washthe combined organic extracts were washed with 5% aqueous sodium carbonate
  4. dry with materialdried (potassium carbonate)
  5. customthe solvent was removed in vacuo
  6. customthat obtained from an identical reaction
  7. customwas purified by flash chromatography
  8. washeluting with 2% ethyl acetate/chloroform