Nitrogen → 1-Chloro-4-ethyl-6-methoxy-phthalazine

HRID 2268833Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2268833
[CH2:1]([C:3]1[C:12]2[C:7](=[CH:8][CH:9]=[C:10]([O:13][CH3:14])[CH:11]=2)[C:6](=O)[NH:5][N:4]=1)[CH3:2].N#N.P(Cl)(Cl)([Cl:20])=O.C([O-])([O-])=O.[Na+].[Na+]>C(#N)C.O>[Cl:20][C:6]1[C:7]2[C:12](=[CH:11][C:10]([O:13][CH3:14])=[CH:9][CH:8]=2)[C:3]([CH2:1][CH3:2])=[N:4][N:5]=1

Komponenten

7

Edukt 4

HCID 947NitrogenHCID 10340Sodium CarbonateHCID 24813Phosphorus oxychlorideHCID 183816114-ethyl-6-methoxy-2H-phthalazin-1-one

Produkt 1

HCID 183816451-Chloro-4-ethyl-6-methoxy-phthalazineAusbeute 89 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 6342AcetonitrileLösungsmittel

Versuchsvorschrift

A suspension of 4-ethyl-6-methoxy-2H-phthalazin-1-one (1.3 g, 6.76 mmoles), prepared as described in example 9, in dry acetonitrile (20 ml), under stirring and dry N2 at room temperature, was added with phosphorous oxychloride (2.07 g, 13.52 mmoles). The mixture was refluxed and after 2 hours cooled, brought to small volume, taken up in water, added with Na2CO3 in excess and extracted three times with CH2Cl2. The organic phases were anhydrified and brought to dryness to give 1.34 g of the title compound (yield: 89%).

Aufarbeitung

  1. customprepared
  2. temperatureThe mixture was refluxed and after 2 hours
  3. temperaturecooled
  4. extractionextracted three times with CH2Cl2

Quellen und Nachweise

ORD-Eintrag
ord-687c15e315844155ac11d7ef40e0aae8
Quelldatensatz
uspto-grants-2001_12
Patentnummer
US06329370B1

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