Hydrochloric Acid → 4-(Hydrazinocarbonyl)benzoic acid

HRID 973537

Reaktionsgleichung

Reaktionsgleichung von HRID 973537
[C:1]([O:12]C)(=[O:11])[C:2]1[CH:10]=[CH:9][C:5]([C:6]([O-])=[O:7])=[CH:4][CH:3]=1.O.[NH2:15][NH2:16].Cl>CO>[C:1]([C:2]1[CH:10]=[CH:9][C:5]([C:6]([NH:15][NH2:16])=[O:7])=[CH:4][CH:3]=1)([OH:12])=[O:11]

Komponenten

5

Edukt 3

HCID 313Hydrochloric AcidHCID 24654Hydrazine hydrate (1:1)HCID 36144541,4-Benzenedicarboxylic acid, methyl ester

Produkt 1

HCID 2794374-(Hydrazinocarbonyl)benzoic acid

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

In 1 l of methanol was dissolved 180 g of monomethyl terephthalate, and the solution was slowly added dropwise to 500 ml of hydrazine hydrate (50%) at room temperature while stirring. After the drop-wise addition, the mixture was heat-refluxed for 5 hours while stirring. A hydrochloric acid aqueous solution was slowly added to the reaction mixture to adjust to a pH of about 1 to thereby precipitate white crystals. Two liters of water was added to the system, followed by stirring for a while. The formed crystals were collected by filtration under reduced pressure, washed twice with 200 ml of water, and dried to obtain 160 g of p-carboxybenzhydrazide (melting point: 235-236° C.).

Aufarbeitung

  1. additionAfter the drop-wise addition
  2. temperaturethe mixture was heat-refluxed for 5 hours
  3. stirringwhile stirring
  4. customto thereby precipitate white crystals
  5. additionTwo liters of water was added to the system
  6. stirringby stirring for a while
  7. filtrationThe formed crystals were collected by filtration under reduced pressure
  8. washwashed twice with 200 ml of water
  9. customdried

Quellen und Nachweise

ORD-Eintrag
ord-fdb0439c7795491b846d322bb06d0045
Quelldatensatz
uspto-grants-1991_11
Patentnummer
US05064751

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