反応 #94952

反応方程式

1-(phenylmethyl)-4-piperidinecarbonitrile

ammonium chloride

water

magnesium

1-bromo-2-methylbenzene

→

(2-methylphenyl) [1-(phenylmethyl)-4-piperidinyl]methanone

溶媒

1,1'-oxybisethane

1,1'-oxybisethane

反応条件

後処理

1. 1
   温度is refluxing
2. 2
   温度at reflux
3. 3
   workup.STIRRINGUpon completion, stirring
4. 4
   workup.WAITis continued for 4 hours at room temperature
5. 5
   その他The organic phase is separated
6. 6
   その他dried
7. 7
   ろ過filtered
8. 8
   その他evaporated

実験手順

To 7 parts of magnesium is added dropwise a solution of 50 parts of 1-bromo-2-methylbenzene in 140 parts of 1,1'-oxybisethane so that the mixture is refluxing. The whole is stirred for 15 minutes at reflux. The Grignard-complex is cooled to 10° C. and there is added dropwise a solution of 30 parts of 1-(phenylmethyl)-4-piperidinecarbonitrile in 70 parts of 1,1'-oxybisethane. Upon completion, stirring is continued for 4 hours at room temperature. The reaction mixture is decomposed with a solution of 40 parts of ammonium chloride in 400 parts of water. The organic phase is separated, dried, filtered and evaporated, yielding 31 parts of (2-methylphenyl) [1-(phenylmethyl)-4-piperidinyl]methanone as an oily residue.

出典