6-fluoro-3-[4-(phenylmethyl)piperazinyl]-1H-indazole → 6-fluoro-3-piperazin-1-yl-1H-indazole

HRID 2051013Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2051013
[F:1][C:2]1[CH:10]=[C:9]2[C:5]([C:6]([N:11]3[CH2:16][CH2:15][N:14](CC4C=CC=CC=4)[CH2:13][CH2:12]3)=[N:7][NH:8]2)=[CH:4][CH:3]=1.[H][H]>[Ni].[Pd].CO>[F:1][C:2]1[CH:10]=[C:9]2[C:5]([C:6]([N:11]3[CH2:12][CH2:13][NH:14][CH2:15][CH2:16]3)=[N:7][NH:8]2)=[CH:4][CH:3]=1

Komponenten

6

Edukt 2

HCID 150574536-fluoro-3-[4-(phenylmethyl)piperazinyl]-1H-indazoleHCID 178418361HCID 178418361, Verbindung

Produkt 1

HCID 98158716-fluoro-3-piperazin-1-yl-1H-indazoleAusbeute 92 %

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 935NickelKatalysatorHCID 23938PalladiumKatalysatorHCID 887MethanolLösungsmittel

Versuchsvorschrift

A mixture of 12 parts of 6-fluoro-3-[4-(phenylmethyl)-piperazinyl]-1H-indazole, 1 part of Raney nickel catalyst and 200 parts of methanol was hydrogenated in a Parr-apparatus at normal pressure and at 50° C. with 2 parts of palladium-on-charcoal catalyst 10%. After the calculated amount of hydrogen was taken up, the catalyst was filtered off over diatomaceous earth and the filtrate was evaporated in vacuo. The residue was crystallized from acetonitrile. The product was filtered off and dried, yielding 7.7 parts (92.0%) of 6-fluoro-3-(1-piperazinyl)-1H-indazole (int. 8).

Aufarbeitung

  1. filtrationthe catalyst was filtered off over diatomaceous earth
  2. customthe filtrate was evaporated in vacuo
  3. customThe residue was crystallized from acetonitrile
  4. filtrationThe product was filtered off
  5. customdried

Quellen und Nachweise

ORD-Eintrag
ord-e917cc2fee1b4d01aa6d2c9be5496036
Quelldatensatz
uspto-grants-1991_05
Patentnummer
US05015740

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