반응 #93468

반응 방정식

2-chloropyrimidine

1-(6-benzodioxinyl methyl)piperazine

potassium carbonate

→

1-(benzodioxin-6-yl methyl)-4-(pyrimidin-2-yl)piperazine dihydrochloride

수율 156.5%

용매

pentanol

반응 조건

후처리

1. 1
   기타After the completion of the reaction
2. 2
   여과the so-formed salt was filtered off
3. 3
   기타the solvent was evaporated under reduced pressure
4. 4
   workup.DISSOLUTIONThe so-obtained oily residue (30 g) was dissolved in 160 ml of anhydrous ethanol
5. 5
   workup.ADDITIONAfter addition of an excess of hydrochloric acid ether solution
6. 6
   기타the dihydrochloride crystallises

실험 절차

A solution of 11.4 g (0.1 mole) of 2-chloropyrimidine and 23.2 g (0.1 mole) of 1-(6-benzodioxinyl methyl)piperazine (oil) in 500 ml of pentanol, as refluxed for 6 hours, in the presence of 13.8 g (0.1 mole) of potassium carbonate. After the completion of the reaction, the so-formed salt was filtered off and the solvent was evaporated under reduced pressure. The so-obtained oily residue (30 g) was dissolved in 160 ml of anhydrous ethanol. After addition of an excess of hydrochloric acid ether solution, the dihydrochloride crystallises. 30 g of 1-(benzodioxin-6-yl methyl)-4-(pyrimidin-2-yl)piperazine dihydrochloride white crystals were finally obtained, melting at 215°-220° C.

출처