Ethyl formate → 1-Formyl-4-(4-methoxyphenyl)piperazine
Reaktionsgleichung
[OH2:1].Cl.Cl.C1(C[CH2:15][N:16]2[CH2:21][CH2:20][N:19]([C:22]3[CH:27]=[CH:26][CH:25]=[CH:24][C:23]=3OC)[CH2:18][CH2:17]2)C2C(=CC=CC=2)CCO1.[CH:30](OCC)=[O:31]>>[CH:15]([N:16]1[CH2:17][CH2:18][N:19]([C:22]2[CH:23]=[CH:24][C:25]([O:31][CH3:30])=[CH:26][CH:27]=2)[CH2:20][CH2:21]1)=[O:1]Komponenten
3
Versuchsvorschrift
A mixture of 1-(4-methoxyphenyl)piperazine (XI, 7.41 g) and ethyl formate (108 ml) is stirred at reflux for 3 hr. The mixture is then cooled, concentrated, and the residue chromatographed on silica gel eluting with methanol/dichloromethane (2/98). The appropriate fractions are pooled and concentrated to give 1-formyl-4-(4-methoxyphenyl)piperazine (VI), NMR (CDCl3) δ 3.05, 3.54, 3.71, 3.78, 6.88, 8.10.
Aufarbeitung
- temperatureat reflux for 3 hr
- temperatureThe mixture is then cooled
- concentrationconcentrated