1-Methylpiperazine → HCID 86607093, Verbindung
Reaktionsgleichung
[Br:1][CH2:2][C:3]1[O:4][CH:5]=[C:6]([OH:10])[C:7](=[O:9])[CH:8]=1.[CH3:11][N:12]1[CH2:17][CH2:16][NH:15][CH2:14][CH2:13]1>O1CCCC1>[BrH:1].[OH:10][C:6]1[C:7](=[O:9])[CH:8]=[C:3]([CH2:2][N:15]2[CH2:16][CH2:17][N:12]([CH3:11])[CH2:13][CH2:14]2)[O:4][CH:5]=1Komponenten
4
Edukt 2
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Reaktionsbedingungen
- Temperatur
- 75 °C
Versuchsvorschrift
2-(Bromomethyl)-5-hydroxy-4H-pyran-4-one 21 (0.5 g, 2.4 mmol), 1-methylpiperazine (0.3 mL, 2.4 mmol) and tetrahydrofurane (12 mL) were charged in a 250 ml round-bottomed flask equipped with a magnetic stirrer. The reaction mixture was stirred for 2 h at 75° C. The reaction mixture was cooled and the precipitate was filtered to give after drying 5-hydroxy-2-((4-methylpiperazin-1-yl)methyl)-4H-pyran-4-one hydrobromide 23 (0.6 g, 83% yield) as a beige solid. A cesium salt was prepared by adding to Cs2CO3 (7.3 g, 22.4 mmol) in water (20 mL). The aqueous phase was washed with CH2Cl2 (200 mL), then water was evaporated at 40° C. and the cesium salt was drying under vacuum to give a white powder.