HRID450950

反应详情

EQUATION

反应方程式

HRID 450950 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Potassium hydroxide (135 mg, 2.41 mmol) was added to a solution of the product of example 105(53 mg, 0.12 mmol) in 3-methyl-3-pentanol (5 mL) and the mixture was heated under reflux for 18 hours. The reaction mixture was then cooled to room temperature, concentrated in vacuo and the residue was partitioned between ethyl acetate (20 mL) and water (5 mL). The aqueous layer was separated, extracted with ethyl acetate (2×20 mL) and the combined organic solution was dried over magnesium sulfate and concentrated in vacuo to give a colourless oil in 96% yield, 53 mg.

WORKUP

后处理

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 18 hours
  3. concentrationconcentrated in vacuo
  4. customthe residue was partitioned between ethyl acetate (20 mL) and water (5 mL)
  5. customThe aqueous layer was separated
  6. extractionextracted with ethyl acetate (2×20 mL)
  7. dry with materialthe combined organic solution was dried over magnesium sulfate
  8. concentrationconcentrated in vacuo
  9. customto give a colourless oil in 96% yield, 53 mg