反応 #40310

反応方程式

methyl iodide

potassium hydride

2-methylcyclohexanone

Triethylborane

→

title compound

2,2-dimethyl-cyclohexanone

溶媒

tetrahydrofuran

反応条件

後処理

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

実験手順

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).

出典