Reaktionsgleichung
[N+:1]([C:4]1[CH:11]=[CH:10][CH:9]=[CH:8][C:5]=1[CH:6]=[O:7])([O-:3])=O.[CH3:12][CH:13]1[CH2:18][C:17](=[O:19])[CH2:16][C:15](=O)[CH2:14]1.[ClH:21].O>O1CCCC1>[Cl:21][C:9]1[CH:8]=[C:5]2[C:4]([N:1]([OH:3])[C:15]3[CH2:14][CH:13]([CH3:12])[CH2:18][C:17](=[O:19])[C:16]=3[C:6]2=[O:7])=[CH:11][CH:10]=1Komponenten
6
Edukt 4
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Versuchsvorschrift
30.2 g (0.2 mole) of 2-nitrobezaldehyde and 25.2 g (0.2 mole) of 5-methyl-1,3-cyclohexane-dione were dissolved in 300 ml of tetrahydrofurane, the solution was saturated at 18° C with hydrogen chloride and allowed to stand for 4 days at room temperature. Water was added, the oily layer was separated and stirred with methanol. The crystals that had formed were filtered off, washed with methanol and dissolved and recrystallized from glacial acetic acid. 9.5 g (17 % of the theory) of 7-chloro-3-methyl-10-hydroxy-1-oxo-1,2,3,4-tetrahydro-9(10H)-acridone having a decomposition point of 255° C were obtained.
Aufarbeitung
- customthe oily layer was separated
- customThe crystals that had formed
- filtrationwere filtered off
- washwashed with methanol
- dissolutiondissolved
- customrecrystallized from glacial acetic acid
Quellen und Nachweise
- ORD-Eintrag
- ord-b7b28e330e6243c899d66b4fb4eab0ff
- Quelldatensatz
- uspto-grants-1976_03
- Patentnummer
- US03947449
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