Hexamethylenetetramine → HCID 21919188, Verbindung
Reaktionsgleichung
[CH3:1][O:2][C:3]1[C:4]([CH3:23])=[C:5]([C:14]([O:21][CH3:22])=[C:15]([O:19][CH3:20])[C:16]=1[O:17][CH3:18])[CH2:6][C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][C:8]=1[OH:13].C1N2CN3CN(C2)CN1C3.FC(F)(F)[C:36](O)=[O:37]>>[CH3:1][O:2][C:3]1[C:4]([CH3:23])=[C:5]([C:14]([O:21][CH3:22])=[C:15]([O:19][CH3:20])[C:16]=1[O:17][CH3:18])[CH2:6][C:7]1[C:8]([OH:13])=[C:9]([CH:10]=[CH:11][CH:12]=1)[CH:36]=[O:37]Komponenten
4
Reaktionsbedingungen
- Temperatur
- 80 °C
Versuchsvorschrift
2-(3,4,5,6-Tetramethoxy-2-methylbenzyl)phenol (8.64 g, 27.17 mmol) and hexamethylenetetramine (5.00 g, 35.67 mmol) were dissolved in trifluoroacetic acid (100 ml) followed by heating at 80° C. with stirring for 4 hours. After completion of the reaction, the solvent was evaporated therefrom, water (100 ml) was added to the resulting residue and the mixture was stirred for 30 minutes and extracted with methylene chloride. The extract was washed with water and dried, the solvent was evaporated therefrom and the resulting residue was purified by silica gel column chromatography (hexane:ethyl acetate=4:1) to give the title compound (2.50 g, 7.23 mmol, 27%).
Aufarbeitung
- customAfter completion of the reaction
- customthe solvent was evaporated
- additionwater (100 ml) was added to the resulting residue
- stirringthe mixture was stirred for 30 minutes
- extractionextracted with methylene chloride
- washThe extract was washed with water
- customdried
- customthe solvent was evaporated
- customthe resulting residue was purified by silica gel column chromatography (hexane:ethyl acetate=4:1)
Quellen und Nachweise
- ORD-Eintrag
- ord-4ee18b72d32f40eea2ec1086efa3fcba
- Quelldatensatz
- uspto-grants-2006_10
- Patentnummer
- US07122543B2
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