Reaktionsgleichung
[Cl:1][C:2]1[C:3](O)=[CH:4][CH:5]=[C:6]2[C:11]=1[CH:10]=[N:9][CH:8]=[C:7]2[CH3:12].[Cl:14]P(Cl)(C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1>>[Cl:14][C:3]1[C:2]([Cl:1])=[C:11]2[C:6]([C:7]([CH3:12])=[CH:8][N:9]=[CH:10]2)=[CH:5][CH:4]=1Komponenten
3
Versuchsvorschrift
8-Chloro-7-hydroxy-4-methylisoquinoline (0.04 mole) and dichlorotriphenylphosphorane (0.04 mole) are heated to 240° C. under a nitrogen atmosphere. After 4 hours, the mixture is allowed to cool and is partitioned between chloroform and concentrated hydrochloric acid. The acidic extract is washed with chloroform, basified and extracted with chloroform. The chloroform extract is washed with water, dried over sodium sulfate and evaporated to yield 7,8-dichloro-4-methylisoquinoline. The product is purified by chromatography on silica gel eluted with chloroform and finally by precipitation of the hydrochloride from ethanol-ether.
Aufarbeitung
- temperatureto cool
- customis partitioned between chloroform and concentrated hydrochloric acid
- extractionThe acidic extract
- washis washed with chloroform
- extractionextracted with chloroform
- extractionThe chloroform extract
- washis washed with water
- dry with materialdried over sodium sulfate
- customevaporated
Quellen und Nachweise
- ORD-Eintrag
- ord-664b79f2620b49b5be4c8e1e52b49cab
- Quelldatensatz
- uspto-grants-1976_10
- Patentnummer
- US03988339
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