HRID978994

反应详情

EQUATION

反应方程式

HRID 978994 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Iodotrimethylsilane (0.3 ml) was added to a solution of 2-butyryl-3-hydroxy-5-(3-methoxymethyl-2,4,6-trimethylphenyl)cyclohex-2-en-1-one (0.5 g, 1.45 mmole) (see Example 36) in dry acetonitrile (10 ml) under nitrogen and the mixture was stirred at room temperature for 15 minutes. An aqueous solution of silver nitrate was added and the mixture was stirred for a further 4 hours. The solvent was evaporated and the residue was washed successively with dilute aqueous sodium hydroxide and acetic acid, then dissolved in ethyl acetate and dried over anhydrous sodium sulfate. Evaporation under reduced pressure yielded 2-butyryl-3-hydroxy-5-(3-hydroxymethyl-2,4,6-trimethylphenyl)cyclohex-2-en-1-one (0.42 g; 87.0%) as an oil.

WORKUP

后处理

  1. stirringthe mixture was stirred for a further 4 hours
  2. customThe solvent was evaporated
  3. washthe residue was washed successively with dilute aqueous sodium hydroxide and acetic acid
  4. dissolutiondissolved in ethyl acetate
  5. dry with materialdried over anhydrous sodium sulfate
  6. customEvaporation under reduced pressure