2-[1-(1-Methoxycarbonylpiperidin-4-yl)-piperidin-4-yl]amino-3-nitropyridine → 3-Amino-2-[1-(1-methoxycarbonylpiperidin-4-yl)-piperidin-4-yl]aminopyridin

HRID 47533Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 47533
[CH3:1][O:2][C:3]([N:5]1[CH2:10][CH2:9][CH:8]([N:11]2[CH2:16][CH2:15][CH:14]([NH:17][C:18]3[C:23]([N+:24]([O-])=O)=[CH:22][CH:21]=[CH:20][N:19]=3)[CH2:13][CH2:12]2)[CH2:7][CH2:6]1)=[O:4].[H][H]>CO.[Pd]>[NH2:24][C:23]1[C:18]([NH:17][CH:14]2[CH2:15][CH2:16][N:11]([CH:8]3[CH2:9][CH2:10][N:5]([C:3]([O:2][CH3:1])=[O:4])[CH2:6][CH2:7]3)[CH2:12][CH2:13]2)=[N:19][CH:20]=[CH:21][CH:22]=1

Komponenten

5

Edukt 2

HCID 178310772-[1-(1-Methoxycarbonylpiperidin-4-yl)-piperidin-4-yl]amino-3-nitropyridineHCID 178418361HCID 178418361, Verbindung

Produkt 1

HCID 227452603-Amino-2-[1-(1-methoxycarbonylpiperidin-4-yl)-piperidin-4-yl]aminopyridin

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 23938PalladiumKatalysatorHCID 887MethanolLösungsmittel

Versuchsvorschrift

Seventy (70) mg of 2-[1-(1-methoxycarbonylpiperidin-4-yl)-piperidin-4-yl]amino-3-nitropyridine was dissolved in 5 ml of methanol, and to which 20 mg of 10% palladium/carbon catalyst was added to effect catalytic reduction at room temperature under atmospheric pressure of hydrogen. After filtering the catalyst off and drying the filtrate to solid, the resulting residue was purified by silica gel column chromatography (chloroform/methanol=95/5) to give 20 mg of 3-amino-2-[1-(1-methoxycarbonylpiperidin-4-yl)-piperidin-4-yl]aminopyridin.

Aufarbeitung

  1. customat room temperature
  2. filtrationAfter filtering the catalyst off and
  3. customdrying the filtrate to solid
  4. customthe resulting residue was purified by silica gel column chromatography (chloroform/methanol=95/5)

Quellen und Nachweise

ORD-Eintrag
ord-3c753ad01d3a4689adf159fe655e9a2f
Quelldatensatz
uspto-grants-2004_03
Patentnummer
US06699880B1

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