Hydrazine hydrate (1:1) → [4-(3,5-Dichloro-pyridin-4-ylmethyl)-7-methoxy-phthalazin-1-yl]-hydrazine

HRID 1060585Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1060585
O.[NH2:2][NH2:3].Cl[C:5]1[C:14]2[C:9](=[CH:10][CH:11]=[C:12]([O:15][CH3:16])[CH:13]=2)[C:8]([CH2:17][C:18]2[C:23]([Cl:24])=[CH:22][N:21]=[CH:20][C:19]=2[Cl:25])=[N:7][N:6]=1>C(O)C>[Cl:25][C:19]1[CH:20]=[N:21][CH:22]=[C:23]([Cl:24])[C:18]=1[CH2:17][C:8]1[C:9]2[C:14](=[CH:13][C:12]([O:15][CH3:16])=[CH:11][CH:10]=2)[C:5]([NH:2][NH2:3])=[N:6][N:7]=1

Komponenten

4

Edukt 2

HCID 24654Hydrazine hydrate (1:1)HCID 186292104-Chloro-1-[(3,5-dichloropyridin-4-yl)methyl]-6-methoxyphthalazine

Produkt 1

HCID 18629212[4-(3,5-Dichloro-pyridin-4-ylmethyl)-7-methoxy-phthalazin-1-yl]-hydrazineAusbeute 109,1 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

Hydrazine hydrate (0.81 ml, 0.84 g, 16.8 mmoles) was added to a solution under N2 of 4-chloro-1-(3,5-dichloro-pyridin-4-ylmethyl)-6-methoxy-phthalazine (2 g, 5.6 mmoles), obtained as described in example 13, in ethanol (30 ml), and the mixture was kept under reflux for 24 hours, then cooled in ice and the resultant precipitate was filtered, washed with ethanol and ethyl ether and dried under vacuum at 50° C. to give 2.14 g of the title compound (stoichiometric yield). m.p.: 297-299° C.

Aufarbeitung

  1. customobtained
  2. temperatureunder reflux for 24 hours
  3. temperaturecooled in ice
  4. filtrationthe resultant precipitate was filtered
  5. washwashed with ethanol and ethyl ether
  6. customdried under vacuum at 50° C.

Quellen und Nachweise

ORD-Eintrag
ord-a80c100b29034a9caab5a688b6c27a70
Quelldatensatz
uspto-grants-2003_02
Patentnummer
US06525055B1

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