Triphenylphosphine dichloride → HCID 21393849, Verbindung

HRID 461506

Reaktionsgleichung

Reaktionsgleichung von HRID 461506
[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]=1

Komponenten

3

Edukt 2

HCID 260420Triphenylphosphine dichlorideHCID 21393806HCID 21393806, Verbindung

Produkt 1

HCID 21393849HCID 21393849, Verbindung

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 four 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

  1. temperatureto cool
  2. customis partitioned between chloroform and concentrated hydrochloric acid
  3. extractionThe acidic extract
  4. washis washed with chloroform
  5. extractionextracted with chloroform
  6. extractionThe chloroform extract
  7. washis washed with water
  8. dry with materialdried over sodium sulfate
  9. customevaporated

Quellen und Nachweise

ORD-Eintrag
ord-5b22cc1d06044d2b8335d8b22366d2ad
Quelldatensatz
uspto-grants-1977_12
Patentnummer
US04062961

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