Hydrochloric Acid → 3-Nitrobenzohydrazide

HRID 267176

Reaktionsgleichung

Reaktionsgleichung von HRID 267176
[N+:1]([C:4]1[CH:5]=[C:6]([CH:10]=[CH:11][CH:12]=1)[C:7](O)=[O:8])([O-:3])=[O:2].Cl.O.[NH2:15][NH2:16]>CO>[N+:1]([C:4]1[CH:5]=[C:6]([CH:10]=[CH:11][CH:12]=1)[C:7]([NH:15][NH2:16])=[O:8])([O-:3])=[O:2]

Komponenten

5

Edukt 3

HCID 313Hydrochloric AcidHCID 84973-Nitrobenzoic acidHCID 24654Hydrazine hydrate (1:1)

Produkt 1

HCID 32914983-Nitrobenzohydrazide

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

A mixture of 167g (1 mole) of m-nitrobenzoic acid and 160g (5 moles) of methanol was refluxed with stirring for 3 hours while a stream of dry HCl was bubbled in. A precipitate which formed on cooling to room temperature was filtered off, and dissolved in hot methanol. The solution was boiled for 10 minutes with a mixture of sodium carbonate and anhydrous calcium sulfate and was then filtered. The filtrate was stirred and refluxed while 118g (2 moles) of 85% hydrazine hydrate was added. The mixture was refluxed for 90 minutes and allowed to cool. The solid product was filtered off and recrystallized from water to give 258 g of m-nitrobenzhydrazide, m.p. 155°-155.5°C.

Aufarbeitung

  1. temperaturewas refluxed
  2. customwas bubbled in
  3. customA precipitate which formed
  4. filtrationwas filtered off
  5. dissolutiondissolved in hot methanol
  6. additionThe solution was boiled for 10 minutes with a mixture of sodium carbonate and anhydrous calcium sulfate
  7. filtrationwas then filtered
  8. additionwas added
  9. temperatureThe mixture was refluxed for 90 minutes
  10. temperatureto cool
  11. filtrationThe solid product was filtered off
  12. customrecrystallized from water

Quellen und Nachweise

ORD-Eintrag
ord-6b28c221ca384031a8a33b4f05e7d3a8
Quelldatensatz
uspto-grants-1976_03
Patentnummer
US03941749

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