Sodium Hydroxide → HCID 69859166, Verbindung

HRID 1456319Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1456319
[N+:1]([C:4]1[C:5]([C:10]2[CH:15]=[CH:14][C:13]([CH3:16])=[CH:12][CH:11]=2)=[N:6][CH:7]=[CH:8][CH:9]=1)([O-])=O.[H][H].[OH-].[Na+]>C(O)C.Cl>[C:13]1([CH3:16])[CH:12]=[CH:11][C:10]([C@H:5]2[C@@H:4]([NH2:1])[CH2:9][CH2:8][CH2:7][NH:6]2)=[CH:15][CH:14]=1

Komponenten

6

Edukt 3

HCID 14798Sodium HydroxideHCID 11241348HCID 11241348, VerbindungHCID 178418361HCID 178418361, Verbindung

Produkt 1

HCID 69859166HCID 69859166, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 313Hydrochloric AcidLösungsmittelHCID 702EthanolLösungsmittel

Versuchsvorschrift

A stirred solution of 3-nitro-2-p-tolylpyridine (5.0 g) in ethanol (200 ml) and concentrated hydrochloric acid (15 ml) was hydrogenated over pre-reduced platinum oxide (1.5 g) at 23°1 atm until hydrogen uptake was complete (~3 lh). The mixture was filtered through hyflo washing the pad of hyflo with water then the filtrate was evaporated in vacuo. Recrystallisation from isopropanol water gave a cream solid. The solid was treated with 2N sodium hydroxide solution and extracted with dichloromethane (5×200 ml). The combined organic extracts were dried (Na2SO4) and evaporated in vacuo to give the title compound as an orange-brown oil which partially crystallised on standing (2.20 g).

Aufarbeitung

  1. filtrationThe mixture was filtered through hyflo
  2. washwashing the pad of hyflo with water
  3. customthe filtrate was evaporated in vacuo
  4. customRecrystallisation from isopropanol water
  5. customgave a cream solid
  6. extractionextracted with dichloromethane (5×200 ml)
  7. dry with materialThe combined organic extracts were dried (Na2SO4)
  8. customevaporated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-2a46ad45f7984c92951b5851a3a48050
Quelldatensatz
uspto-grants-1998_12
Patentnummer
US05843966

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