反応 #94951

反応方程式

iodine

4-chloro-1-methylpiperidine

3-methylbenzonitrile

magnesium

1,2-dibromoethane

ammonium chloride

water

→

(3-methylphenyl) (1-methyl-4-piperidinyl)methanone

溶媒

tetrahydrofuran

tetrahydrofuran

反応条件

後処理

1. 1
   その他the reaction
2. 2
   温度After cooling
3. 3
   温度at reflux temperature
4. 4
   温度The reaction mixture is cooled
5. 5
   抽出The product is extracted with 2,2'-oxybispropane
6. 6
   洗浄The extract is washed with water
7. 7
   その他dried
8. 8
   ろ過filtered
9. 9
   その他evaporated

実験手順

To 5 parts of magnesium are added 2.18 parts of 1,2-dibromoethane and a small amount of iodine to initiate the reaction. Then there is added dropwise a solution of 28 parts of 4-chloro-1-methylpiperidine in 180 parts of tetrahydrofuran while the mixture is heated to 70° C. After cooling, there is added dropwise a solution of 14 parts of 3-methylbenzonitrile in 90 parts of tetrahydrofuran. Upon completion, stirring is continued for 1 hour at reflux temperature. The reaction mixture is cooled and poured onto a solution of 75 parts of ammonium chloride in water. The product is extracted with 2,2'-oxybispropane. The extract is washed with water, dried, filtered and evaporated, yielding 35 parts of (3-methylphenyl) (1-methyl-4-piperidinyl)methanone as an oily residue.

出典