反応 #65040

反応方程式

1,12-dibromododecane

N-phenylpiperazine

triethylamine

toluene

→

1-bromo-12-(4-phenylpiperazinyl)dodecane

収率 50.1%

溶媒

ethyl acetate

反応条件

後処理

1. 1
   温度was heated
2. 2
   温度under reflux for 2 hours
3. 3
   洗浄the mixture was washed successively with water
4. 4
   乾燥a saturated sodium chloride aqueous solution, and dried over magnesium sulfate
5. 5
   その他The solvent was evaporated under reduced pressure
6. 6
   workup.ADDITIONa 1:2 mixture of ethyl acetate and hexane as a developing solvent

実験手順

A mixture of 6.56 g of 1,12-dibromododecane, 3.24 g of N-phenylpiperazine, 2.53 g of triethylamine, and 50 ml of toluene was heated under reflux for 2 hours. To the reaction mixture was added 100 ml of ethyl acetate, and the mixture was washed successively with water and a saturated sodium chloride aqueous solution, and dried over magnesium sulfate. The solvent was evaporated under reduced pressure, and the residue was subjected to column chromatography using a 1:2 mixture of ethyl acetate and hexane as a developing solvent to yield 4.1 g of 1-bromo-12-(4-phenylpiperazinyl)dodecane (m.p.=26.0°-28.0° C.).

出典