Reaktionsgleichung
[Cl:1][C:2]1[N:7]=[CH:6][CH:5]=[CH:4][N:3]=1.[O:8]1[C:13]2[CH:14]=[CH:15][C:16]([CH2:18][N:19]3[CH2:24][CH2:23][NH:22][CH2:21][CH2:20]3)=[CH:17][C:12]=2[O:11][CH:10]=[CH:9]1.C(=O)([O-])[O-].[K+].[K+]>C(O)CCCC>[ClH:1].[ClH:1].[O:8]1[C:13]2[CH:14]=[CH:15][C:16]([CH2:18][N:19]3[CH2:20][CH2:21][N:22]([C:2]4[N:7]=[CH:6][CH:5]=[CH:4][N:3]=4)[CH2:23][CH2:24]3)=[CH:17][C:12]=2[O:11][CH:10]=[CH:9]1Komponenten
5
Edukt 3
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Versuchsvorschrift
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.
Aufarbeitung
- customAfter the completion of the reaction
- filtrationthe so-formed salt was filtered off
- customthe solvent was evaporated under reduced pressure
- dissolutionThe so-obtained oily residue (30 g) was dissolved in 160 ml of anhydrous ethanol
- additionAfter addition of an excess of hydrochloric acid ether solution
- customthe dihydrochloride crystallises
Quellen und Nachweise
- ORD-Eintrag
- ord-446e8a80fd7642449b2d5bff95ba4b59
- Quelldatensatz
- uspto-grants-1986_09
- Patentnummer
- US04613601
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