HRID1780852

反应详情

EQUATION

反应方程式

HRID 1780852 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

A solution of 4-cyano-4-(3-cyclopentyloxy-4-methoxyphenyl)cyclohexan-1-one dimethyl ketal (0.34 g, 0.95 mmol) and powdered potassium carbonate (0.7 g, 5.1 mmol) in methanol (20 mL) and water (4 mL) at 0° C. was treated with hydrogen peroxide (30% solution, 2.55 mL). The mixture was allowed to warm to room temperature and, after seven days, brine was added and the mixture was extracted with methylene chloride. The organic extract was washed twice with brine, dried (potassium carbonate) and the solvent was removed in vacuo. Purification by flash chromatography provided the amide (0.055 g, 15%) along with recovered starting material (0.25 g).

WORKUP

后处理

  1. extractionthe mixture was extracted with methylene chloride
  2. extractionThe organic extract
  3. washwas washed twice with brine
  4. dry with materialdried (potassium carbonate)
  5. customthe solvent was removed in vacuo
  6. customPurification by flash chromatography