Reaktionsgleichung
[Cl:1][C:2]1[CH:15]=[CH:14][C:5]2[C:6]3[CH2:7][CH2:8][CH2:9][NH:10][C:11]=3[CH2:12][CH2:13][C:4]=2[CH:3]=1.[C:16]1(=[O:32])[N:20]([CH2:21][CH2:22][CH2:23][C:24](Cl)=[O:25])[C:19](=[O:27])[C:18]2=[CH:28][CH:29]=[CH:30][CH:31]=[C:17]12>C(Cl)Cl>[Cl:1][C:2]1[CH:15]=[CH:14][C:5]2[C:6]3[CH2:7][CH2:8][CH2:9][N:10]([C:24](=[O:25])[CH2:23][CH2:22][CH2:21][N:20]4[C:16](=[O:32])[C:17]5=[CH:31][CH:30]=[CH:29][CH:28]=[C:18]5[C:19]4=[O:27])[C:11]=3[CH2:12][CH2:13][C:4]=2[CH:3]=1Komponenten
4
Versuchsvorschrift
31.4 g (0.143 mol) of 8-chloro-1,2,3,4,5,6-hexahydrobenzo[f]quinoline dissolved in 300 ml of methylene chloride are added at 0° to a solution of 36.0 g (0.143 mol) of 4-phthalimidobutyryl chloride in 360 ml of methylene chloride and the mixture is stirred at room temperature for 1 hour. The solution is concentrated, extracted with methylene chloride and aqueous sodium hydrogen carbonate solution dried with magnesium sulfate and the solvent is distilled in a vacuum. Extractive crystallization with acetone gives 8-chloro-1,2,3,4,5,6-hexahydro-4-(4-phthalimidobutyryl)benzo[f]quinoline as white crystals with melting point 182-183°.
Aufarbeitung
- concentrationThe solution is concentrated
- extractionextracted with methylene chloride and aqueous sodium hydrogen carbonate solution
- dry with materialdried with magnesium sulfate
- distillationthe solvent is distilled in a vacuum
- customExtractive crystallization with acetone
Quellen und Nachweise
- ORD-Eintrag
- ord-1b85948fc88c4ba087be929b274b3292
- Quelldatensatz
- uspto-grants-1991_05
- Patentnummer
- US05017608
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