3-(2-Methoxy-pyridin-4-yl)-5-nitro-1-trityl-1H-indazole → 3-(2-methoxypyridin-4-yl)-1-trityl-1H-indazol-5-ylamine

HRID 1020947Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1020947
[CH3:1][O:2][C:3]1[CH:8]=[C:7]([C:9]2[C:17]3[C:12](=[CH:13][CH:14]=[C:15]([N+:18]([O-])=O)[CH:16]=3)[N:11]([C:21]([C:34]3[CH:39]=[CH:38][CH:37]=[CH:36][CH:35]=3)([C:28]3[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=3)[C:22]3[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=3)[N:10]=2)[CH:6]=[CH:5][N:4]=1>CO.C1(C)C=CC=CC=1.[Pd]>[CH3:1][O:2][C:3]1[CH:8]=[C:7]([C:9]2[C:17]3[C:12](=[CH:13][CH:14]=[C:15]([NH2:18])[CH:16]=3)[N:11]([C:21]([C:22]3[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=3)([C:34]3[CH:35]=[CH:36][CH:37]=[CH:38][CH:39]=3)[C:28]3[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=3)[N:10]=2)[CH:6]=[CH:5][N:4]=1

Komponenten

4

Edukt 1

HCID 673446273-(2-Methoxy-pyridin-4-yl)-5-nitro-1-trityl-1H-indazole

Produkt 1

HCID 583720003-(2-methoxypyridin-4-yl)-1-trityl-1H-indazol-5-ylamine

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 23938PalladiumKatalysatorHCID 21867641Toluene methanolLösungsmittel

Versuchsvorschrift

To the stirred suspension of 3-(2-Methoxy-pyridin-4-yl)-5-nitro-1-trityl-1H-indazole 4BV (5.125 g, 10.0 mmole) in MeOH/toluene (50 mL/50 mL) was added 10% Pd/C (Degussa type, 0.5 g) at r.t. under dry N2 gas. The mixture was degassed and was stirred under a balloon inflated with H2 gas overnight. The catalyst was filtered through microfiber filter and was washed with MeOH and CH2Cl2. The filtrate was evaporated to dryness and a brown solid 5BV was obtained (5.0 g).

Aufarbeitung

  1. customThe mixture was degassed
  2. custominflated with H2 gas overnight
  3. filtrationThe catalyst was filtered through microfiber
  4. filtrationfilter
  5. washwas washed with MeOH and CH2Cl2
  6. customThe filtrate was evaporated to dryness
  7. customa brown solid 5BV was obtained (5.0 g)

Quellen und Nachweise

ORD-Eintrag
ord-311c9f53991841e99af52dc0f4531318
Quelldatensatz
uspto-grants-2014_05
Patentnummer
US08716483B2

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