반응 #550484

반응 방정식

1-(4-fluorophenyl)piperazine

cyclopropylmethyl chloride

sodium bicarbonate

→

1-(cyclopropylmethyl)-4-(4-fluorophenyl)piperazine dihydrochloride

수율 139.1%

용매

ethanol

반응 조건

후처리

1. 1
   온도The mixture is kept refluxing for 7 hours
2. 2
   온도After having been cooled
3. 3
   여과the reaction mixture is freed from inorganic matters by filtration
4. 4
   농축the filtrate is concentrated in vacuo
5. 5
   workup.DISSOLUTIONThe residue is dissolved in diethyl ether
6. 6
   workup.ADDITIONgaseous hydrogen chloride is introduced into the solution
7. 7
   온도while being cooled
8. 8
   기타to precipitate crystals which
9. 9
   여과are collected by filtration
10. 10
    기타Upon recrystallization from ethanol

실험 절차

To 50 ml of ethanol, are added 3.6 g (0.02 mole) of 1-(4-fluorophenyl)piperazine, 2.0 g (0.022 mole) of cyclopropylmethyl chloride, and 1.9 g (0.023 mole) of sodium bicarbonate. The mixture is kept refluxing for 7 hours while being stirred. After having been cooled, the reaction mixture is freed from inorganic matters by filtration and the filtrate is concentrated in vacuo. The residue is dissolved in diethyl ether and gaseous hydrogen chloride is introduced into the solution, while being cooled, to precipitate crystals which are collected by filtration. Upon recrystallization from ethanol there are obtained 4.7 g (77% yield) of 1-(cyclopropylmethyl)-4-(4-fluorophenyl)piperazine dihydrochloride melting at 153°-154° C.

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