Hydrazine hydrate (1:1) → 4-(3,5-Dichloro-pyridin-4-ylmethyl)-7-methoxy-2H-phthalazin-1-one

HRID 2268855Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2268855
[Cl:1][C:2]1[CH:3]=[N:4][CH:5]=[C:6]([Cl:21])[C:7]=1[CH:8]=[C:9]1[C:17]2[C:12](=[CH:13][C:14]([O:18][CH3:19])=[CH:15][CH:16]=2)[C:11](=O)[O:10]1.O.[NH2:23][NH2:24]>CO>[Cl:1][C:2]1[CH:3]=[N:4][CH:5]=[C:6]([Cl:21])[C:7]=1[CH2:8][C:9]1[C:17]2[C:12](=[CH:13][C:14]([O:18][CH3:19])=[CH:15][CH:16]=2)[C:11](=[O:10])[NH:24][N:23]=1

Komponenten

4

Edukt 2

HCID 24654Hydrazine hydrate (1:1)HCID 54395392HCID 54395392, Verbindung

Produkt 1

HCID 224827114-(3,5-Dichloro-pyridin-4-ylmethyl)-7-methoxy-2H-phthalazin-1-oneAusbeute 80 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

A suspension of 3-(3,5-dichloro-pyridin-4-ylmethylene)-6-methoxy-3H-isobenzofuran-1-one (84.4 g, 0.126 mole), prepared as described in example 37, in CH3OH (200 ml) under N2 was added with hydrazine monohydrate (18.4 ml, 0.378 mole). The mixture was refluxed for 1 hour, then left overnight at room temperature and cooled over ice. The solid was filtered, washed with cold CH3OH and dried in oven at 50° C. under vacuum; 33.3 g of the title compound were thus obtained (yield: 80%). m.p.: 259-262° C.

Aufarbeitung

  1. customprepared
  2. temperatureThe mixture was refluxed for 1 hour
  3. temperaturecooled over ice
  4. filtrationThe solid was filtered
  5. washwashed with cold CH3OH
  6. customdried in oven at 50° C. under vacuum

Quellen und Nachweise

ORD-Eintrag
ord-de5bc3bb59bf45efa7f95d7cfc09dd6f
Quelldatensatz
uspto-grants-2001_12
Patentnummer
US06329370B1

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