反応 #4413

反応方程式

1-(1-phenylethyl)piperazine

1-bromo-3-chloropropane

→

1,3-bis[4-(1-phenylethyl) -1-piperazinyl]propane tetrahydrochloride

溶媒

ethanol

反応条件

後処理

1. 1
   温度was refluxed for 5 hours
2. 2
   その他The solvent was then removed under vacuum, 75 ml of water
3. 3
   workup.ADDITIONwere added
4. 4
   抽出the mixture was extracted with ether (3×150 ml)
5. 5
   抽出The ether extract
6. 6
   その他was evaporated to an oil
7. 7
   その他chromatographed on silica
8. 8
   workup.DISSOLUTIONThe resulting yellow oil was dissolved in 150 ml of ether
9. 9
   その他precipitated with excess anhydrous hydrogen chloride

実験手順

A mixture of 7.6 g of 1-(1-phenylethyl)piperazine, 3.2 g of 1-bromo-3-chloropropane and 50 ml of reagent ethanol was refluxed for 5 hours. The solvent was then removed under vacuum, 75 ml of water were added, and the mixture was extracted with ether (3×150 ml). The ether extract was evaporated to an oil and chromatographed on silica, the eluant being CH2Cl2 /CH3OH/ammonium hydroxide (45:5:1). The resulting yellow oil was dissolved in 150 ml of ether and precipitated with excess anhydrous hydrogen chloride to yield 6.1 g (51% of theory) of 1,3-bis[4-(1-phenylethyl) -1-piperazinyl]propane tetrahydrochloride. The product was recrystallized from ethanol/water to yield a white crystalline solid (m.p. 236°-246° C., with decomp.).

出典