Dichloromethane → HCID 13560178, Verbindung
Reaktionsgleichung
N#N.CN(C)CCC[C:8]1[CH:13]=[CH:12][N:11]=[C:10]([NH:14][C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)[C:9]=1[NH2:21].[CH2:23]([N:25]([CH2:28][CH3:29])[CH2:26]C)C.[Cl:30][C:31]1[CH:39]=[CH:38][CH:37]=[CH:36][C:32]=1[C:33](Cl)=[O:34].[CH2:40](Cl)Cl>>[Cl:30][C:31]1[CH:39]=[CH:38][CH:37]=[CH:36][C:32]=1[C:33]([NH:21][C:9]1[C:10]([N:14]([CH2:40][CH2:29][CH2:28][N:25]([CH3:23])[CH3:26])[C:15]2[CH:16]=[CH:17][CH:18]=[CH:19][CH:20]=2)=[N:11][CH:12]=[CH:13][CH:8]=1)=[O:34]Komponenten
5
Versuchsvorschrift
To a stirred solution of 9 g (0.033 mole) of N2 -[3-(dimethylamino)propyl]-N2 -phenyl-2,3-pyridinediamine and 3.9 g (0.038 mole) triethylamine in 75 ml of dry methylene chloride was added dropwise with stirring at 15°-20° C., 6.4 g (0.037 mole) of 2-chlorobenzoyl chloride. After stirring overnight, the reaction mixture was washed with water. The methylene chloride layer was extracted twice with dilute sodium hydroxide solution, washed with water, dried over sodium sulfate and concentrated in vacuo. The residue was triturated in isopropyl ether to give 10 g (74%) of solid. A portion of this solid was recrystallized from isopropyl alcohol-isopropyl ether to give a cream colored solid, m.p. 90°-92° C.
Aufarbeitung
- stirringAfter stirring overnight
- washthe reaction mixture was washed with water
- extractionThe methylene chloride layer was extracted twice with dilute sodium hydroxide solution
- washwashed with water
- dry with materialdried over sodium sulfate
- concentrationconcentrated in vacuo
- customThe residue was triturated in isopropyl ether
Quellen und Nachweise
- ORD-Eintrag
- ord-c401ca5e29a34357ab9d199a90f66931
- Quelldatensatz
- uspto-grants-1987_10
- Patentnummer
- US04698430
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