HRID865809

反应详情

EQUATION

反应方程式

HRID 865809 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To the solution obtained as the product of part (ii) was added a solution of potassium permanganate (23 g) in water (260 ml) over 2 hours, keeping the temperature of the reaction below 20° C. 5N hydrochloric acid (30 ml) was then added followed by a solution of sodium metabisulphite (14 g) in water (42 ml). After decolourisation of the mixture the product was extracted into ethyl acetate (250 ml). The organic layer was then concentrated to give an oil. The oil was partitioned between dichloromethane (50 ml) and 2N sodium hydroxide (105 ml) and the organic layer was washed with 5% brine (100 ml). The organic layer was concentrated to give a solution of the title compound which was used directly in the next step.

WORKUP

后处理

  1. customthe temperature of the reaction below 20° C
  2. extractionAfter decolourisation of the mixture the product was extracted into ethyl acetate (250 ml)
  3. concentrationThe organic layer was then concentrated
  4. customto give an oil
  5. customThe oil was partitioned between dichloromethane (50 ml) and 2N sodium hydroxide (105 ml)
  6. washthe organic layer was washed with 5% brine (100 ml)
  7. concentrationThe organic layer was concentrated