2,6-Dimethylaniline → 1,3(2H,4H)-Isoquinolinedione, 2-(2,6-dimethylphenyl)-
Reaktionsgleichung
[C:1]1(=[O:12])[O:7][C:5](=O)[C:4]2=[CH:8][CH:9]=[CH:10][CH:11]=[C:3]2[CH2:2]1.[CH3:13][C:14]1[CH:20]=[CH:19][CH:18]=[C:17]([CH3:21])[C:15]=1[NH2:16]>C(OCC)(=O)C>[CH3:13][C:14]1[CH:20]=[CH:19][CH:18]=[C:17]([CH3:21])[C:15]=1[N:16]1[C:5](=[O:7])[C:4]2=[CH:8][CH:9]=[CH:10][CH:11]=[C:3]2[CH2:2][C:1]1=[O:12]Komponenten
4
Edukt 2
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Versuchsvorschrift
0.67 g (4.13 mmol) of homophthalic anhydride and 0.4 g (3.30 mmol) of 2,6-dimethylaniline were mixed, and melted at a temperature of 200° C. for 1 hour. The reactant was dissolved in ethyl acetate, washed with aqueous NaHCO3 solution, with water and then with saturated aqueous sodium chloride, dried over anhydrous MgSO4, and subjected to filtration with a folded filter paper. The filtrate was concentrated and evaporated to dryness. The residue was recrystallized by using a mixture of CH2Cl2 and hexane, to obtain 0.565 g (yield 68%) of the specified substance as light yellow granulated crystals. It showed the following physical properties and analyzed values.
Aufarbeitung
- washwashed with aqueous NaHCO3 solution, with water
- dry with materialwith saturated aqueous sodium chloride, dried over anhydrous MgSO4
- filtrationsubjected to filtration with a folded filter paper
- concentrationThe filtrate was concentrated
- customevaporated to dryness
- customThe residue was recrystallized
- additiona mixture of CH2Cl2 and hexane
- customto obtain 0.565 g (yield 68%) of the specified substance as light yellow granulated crystals
Quellen und Nachweise
- ORD-Eintrag
- ord-e266e1ecc3c5438cabf5f950025cadeb
- Quelldatensatz
- uspto-grants-2003_02
- Patentnummer
- US06515129B1
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