反应 #64057

反应方程式

Iodotrimethylsilane

2-butyryl-3-hydroxy-5-(3-methoxymethyl-2,4,6-trimethylphenyl)cyclohex-2-en-1-one

→

2-butyryl-3-hydroxy-5-(3-hydroxymethyl-2,4,6-trimethylphenyl)cyclohex-2-en-1-one

收率 87.7%

溶剂

acetonitrile

反应条件

后处理

1. 1
   workup.STIRRINGthe mixture was stirred for a further 4 hours
2. 2
   其他The solvent was evaporated
3. 3
   洗涤the residue was washed successively with dilute aqueous sodium hydroxide and acetic acid
4. 4
   workup.DISSOLUTIONdissolved in ethyl acetate
5. 5
   干燥dried over anhydrous sodium sulfate
6. 6
   其他Evaporation under reduced pressure

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.

来源