Reaktionsgleichung
[CH3:1][N:2]([CH3:31])[C:3]1[CH:8]=[CH:7][C:6]([C:9]2([C:22]3[CH:27]=[CH:26][C:25]([N:28]([CH3:30])[CH3:29])=[CH:24][CH:23]=3)[C:18]3[C:13](=[CH:14][C:15]([N:19]([CH3:21])[CH3:20])=[CH:16][CH:17]=3)[C:11](=[O:12])[O:10]2)=[CH:5][CH:4]=1.CC1C(N)=C(C)C(C)=C(C=1)C(C)(O)C1C=CC(N)=CC=1.CN(C)C1C=C(C=CC=1)C(O)=O>S(=O)(=O)(O)O>[CH3:30][N:28]([CH3:29])[C:25]1[CH:24]=[CH:23][C:22]([CH:9]([C:18]2[CH:17]=[CH:16][C:15]([N:19]([CH3:21])[CH3:20])=[CH:14][C:13]=2[C:11]([OH:12])=[O:10])[C:6]2[CH:5]=[CH:4][C:3]([N:2]([CH3:1])[CH3:31])=[CH:8][CH:7]=2)=[CH:27][CH:26]=1Komponenten
Edukt 3
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Versuchsvorschrift
A process for preparing 3,3-bis(4-dimethylaminophenyl)-6-dimethylaminophthalide which comprises reacting one mole proportion of tetramethyl-4,4'-diaminobenzhydrol with from about 0.9 to about 1.2 mole proportions of 3-dimethylaminobenzoic acid in aqueous sulfuric acid at a temperature of 65°-100° C. to form 2-[4,4'-bis(dimethylamino)benzhydryl]-5-dimethylaminobenzoic acid, adding sodium hydroxide to the reaction mixture to form the sodium salt of the said benzoic acid therein, contacting the reaction mixture at a temperature of about 40°-90° C. with a solvent selected from a liquid aromatic hydrocarbon and a mixture of liquid aromatic hydrocarbon and a water-immiscible alkane, whereby impurities present in said solution are extracted therefrom; separating the organic extract phase from the aqueous reaction mixture phase, treating the reaction mixture phase with an inorganic oxidizing agent to oxidize the sodium salt of the 2-[4,4'-bis(dimethylamino)benzhydryl]-5-dimethylaminobenzoic acid to the 3,3-bis-(4-dimethylaminophenyl)-6-dimethylaminophthalide product and recovering said product from the reaction mixture.
Aufarbeitung
- customat a temperature of 65°-100° C.
Quellen und Nachweise
- ORD-Eintrag
- ord-1138c955bdae4a7d8e83476647acb5f6
- Quelldatensatz
- uspto-grants-1978_02
- Patentnummer
- US04076728
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