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) and the solution was stirred under heating at 80° C. for 4 hours. After the completion of reaction, the solvent was removed by distillation and to the obtained residue, water (100 ml) was added. The resulting solution was stirred for 30 minutes and extracted with methylene chloride. The extract was washed with water and then dried, the solvent was removed by distillation and the obtained residue was purified by silica gel column chromatography (hexand:ethyl acetate=4:1) to obtain the titled compound (2.50 g, 7.23 mmol, 27%).
Aufarbeitung
- customAfter the completion of reaction
- customthe solvent was removed by distillation and to the obtained residue, water (100 ml)
- additionwas added
- stirringThe resulting solution was stirred for 30 minutes
- extractionextracted with methylene chloride
- washThe extract was washed with water
- customdried
- customthe solvent was removed by distillation
- customthe obtained residue was purified by silica gel column chromatography (hexand:ethyl acetate=4:1)
Quellen und Nachweise
- ORD-Eintrag
- ord-dd30e19c2c954e98a9878fb60b997825
- Quelldatensatz
- uspto-grants-2006_06
- Patentnummer
- US07064124B2
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