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Ammonia → HCID 178428768, Verbindung

HRID 1833884
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1833884
Cl[C:2]1[CH:3]=[C:4]([N+:10]([O-:12])=[O:11])[CH:5]=[C:6]([CH3:9])[N+:7]=1[O-:8].[NH3:13]>C(O)C>[NH2:13][C:2]1[CH:3]=[C:4]([N+:10]([O-:12])=[O:11])[CH:5]=[C:6]([CH3:9])[N+:7]=1[O-:8]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 2

HCID 222AmmoniaHCID 27518132-Chloro-6-methyl-4-nitropyridin-N-oxide

Produkt 1

HCID 178428768HCID 178428768, VerbindungAusbeute 41 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

A reaction solution consisting of 5.66 g. (0.03 mole) 6-chloro-4-nitro-2-picoline-1-oxide and 100 ml. ethanol was saturated with anhydrous ammonia and sealed in a strong bottle. This reaction mixture was heated and maintained at a temperature in the range of 100° to 105° C. for 21 hrs. The bottle and contents were then cooled and the seal was broken. Crystals had formed. The crystals were collected on a filter and washed with a small amount of cold ethanol. Recrystallization from 95% aqueous ethanol yielded 2.06 g. (41% yield) of 6-amino-4-nitro-2-picoline-1-oxide as yellow needles having a melting point at 221° to 222° C. (with decomposition). When a small sample was mixed with ethanolic ferric chloride a blue solution was obtained.

Aufarbeitung

  1. customsealed in a strong bottle
  2. temperatureThis reaction mixture was heated
  3. temperaturemaintained at a temperature in the range of 100° to 105° C. for 21 hrs
  4. temperatureThe bottle and contents were then cooled
  5. customCrystals had formed
  6. customThe crystals were collected on
  7. filtrationa filter
  8. washwashed with a small amount of cold ethanol
  9. customRecrystallization from 95% aqueous ethanol
  10. customyielded 2.06 g

Quellen und Nachweise

ORD-Eintrag
ord-aec8dc456b934f14bb77b75163348e90
Quelldatensatz
uspto-grants-1978_01
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04067874

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