反应 #40310

反应方程式

methyl iodide

potassium hydride

2-methylcyclohexanone

Triethylborane

→

title compound

2,2-dimethyl-cyclohexanone

溶剂

tetrahydrofuran

反应条件

后处理

1. 1
   workup.STIRRINGthe mixture is stirred for 16 hours at room temperature
2. 2
   workup.WAITis continued for another 8 hours
3. 3
   其他the reaction is then quenched with saturated aqueous ammonium chloride solution
4. 4
   萃取twice extracted with diethyl ether
5. 5
   干燥The combined organic phases are dried over sodium sulphate
6. 6
   浓缩concentrated to dryness in a vacuum

实验过程

A suspension of potassium hydride (5.5 mmol) and 2-methylcyclohexanone (5 mmol) in dry tetrahydrofuran (10 ml) is stirred for 30 mins at room temperature. Triethylborane (6.25 mmol) is slowly added dropwise and the mixture is stirred for 16 hours at room temperature. After addition of methyl iodide stirring is continued for another 8 hours, the reaction is then quenched with saturated aqueous ammonium chloride solution and twice extracted with diethyl ether. The combined organic phases are dried over sodium sulphate and concentrated to dryness in a vacuum and produce the title compound, which can be reacted without [without] purification (JACS 1985, 107, 19, 5391-5396).

来源