1-[(3,5-dichloropyridin-4-yl)methyl]-6-methoxy-4-phenylphthalazine → HCID 18381610, Verbindung

HRID 2297479Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2297479
[Cl:1][C:2]1[CH:3]=[N:4][CH:5]=[C:6]([Cl:27])[C:7]=1[CH2:8][C:9]1[C:18]2[C:13](=[CH:14][C:15]([O:19][CH3:20])=[CH:16][CH:17]=2)[C:12]([C:21]2[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=2)=[N:11][N:10]=1>C1COCC1.O.[Pt]=O>[Cl:1][C:2]1[CH:3]=[N:4][CH:5]=[C:6]([Cl:27])[C:7]=1[CH2:8][C:9]1[C:18]2[C:13](=[CH:14][C:15]([O:19][CH3:20])=[CH:16][CH:17]=2)[CH:12]([C:21]2[CH:22]=[CH:23][CH:24]=[CH:25][CH:26]=2)[NH:11][N:10]=1

Komponenten

4

Edukt 1

HCID 99525921-[(3,5-dichloropyridin-4-yl)methyl]-6-methoxy-4-phenylphthalazine

Produkt 1

HCID 18381610HCID 18381610, VerbindungAusbeute 32 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 86587499Platinum oxide monohydrateKatalysatorHCID 8028TetrahydrofuranLösungsmittel

Reaktionsbedingungen

Temperatur
50 °C

Versuchsvorschrift

1-(3,5-Dichloro-pyridin-4-ylmethyl)-4-phenyl-6-methoxy-phthalazine (0.5 g, 1.26 mmoles), prepared as described in example 47, in THF (40 ml) was added with platinum oxide hydrate (catalytic amount), then hydrogenated in a Parr at 4 atmospheres under stirring for 4 days and at 50° C. for 24 hours. The catalyst was filtered off and the mixture dried to give a solid which flash chromatographed (eluent: petrolatum/ethyl acetate 8:2) giving 0.16 g of the title compound (yield: 32%). m.p.: 175.3-177.3° C.

Aufarbeitung

  1. filtrationThe catalyst was filtered off
  2. customthe mixture dried
  3. customto give a solid which flash
  4. customchromatographed (eluent: petrolatum/ethyl acetate 8:2)

Quellen und Nachweise

ORD-Eintrag
ord-c544f0cbb59d4f23b3e23e46fd28e4fb
Quelldatensatz
uspto-grants-2002_12
Patentnummer
US06492360B1

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