HRID1163469

反应详情

EQUATION

反应方程式

HRID 1163469 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 15.63 g (100 mmol) of (1R,2S,5R)-2-isopropyl-5-methyl-cyclohexanol and 16.5 g (250 mmol) of potassium hydroxide in 100 ml of N-methylpyrrolidone a solution of 12.73 g (50 mmol) of 2-chloro-1-(4-hydroxy-3,5-di-isopropylphenyl)-ethanone in 400 ml of N-methylpyrrolidone is added dropwise at room temperature and under inert atmosphere. After the addition is completed stirring is continued for additional 16 hours. Then the reaction mixture is acidified with 1N HCl and extracted with ethyl acetate. The collected organic phases are washed with water and brine, dried and evaporated. Crystallization of the crude product from hexane gives 6.37 g of compound 110, m.p. 83-84° C.

WORKUP

后处理

  1. additionAfter the addition
  2. extractionextracted with ethyl acetate
  3. washThe collected organic phases are washed with water and brine
  4. customdried
  5. customevaporated
  6. customCrystallization of the crude product from hexane