Hydrochloric Acid → 3-Fluoro-4-hydroxybenzohydrazide

HRID 1589724Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1589724
[F:1][C:2]1[CH:3]=[C:4]([CH:9]=[CH:10][C:11]=1[OH:12])[C:5](OC)=[O:6].O.[NH2:14][NH2:15].Cl>O>[F:1][C:2]1[CH:3]=[C:4]([CH:9]=[CH:10][C:11]=1[OH:12])[C:5]([NH:14][NH2:15])=[O:6]

Komponenten

5

Edukt 3

HCID 313Hydrochloric AcidHCID 24654Hydrazine hydrate (1:1)HCID 7019368Methyl 3-fluoro-4-hydroxybenzoate

Produkt 1

HCID 109099793-Fluoro-4-hydroxybenzohydrazideAusbeute 92,6 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
100 °C

Versuchsvorschrift

10.00 g (58.8 mM) of methyl 3-fluoro-4-hydroxybenzoate and 17.5 ml of 80%-hydrazine hydrate were mixed and stirred for 1 hour and 20 minutes at 100° C., followed by cooling to room temperature. The resultant mixture was poured into 150 ml of iced water and 16.8 ml of concentrated hydrochloric acid was added thereto (pH=about 8), followed by addition of common salt and stirring at room temperature to precipitate a crystal. The crystal was recovered by filtration and stirred in methanol at room temperature. The resultant crystal was recovered from the above mixture by filtration to obtain 9.26 g of 3-fluoro-4-hydroxybenzohydrazide (Yield: 92.6%).

Aufarbeitung

  1. temperatureby cooling to room temperature
  2. additionwas added
  3. addition(pH=about 8), followed by addition of common salt
  4. stirringstirring at room temperature
  5. customto precipitate a crystal
  6. filtrationThe crystal was recovered by filtration
  7. stirringstirred in methanol at room temperature
  8. filtrationThe resultant crystal was recovered from the above mixture by filtration

Quellen und Nachweise

ORD-Eintrag
ord-99973426cf554ef1ab6281d583d9f09c
Quelldatensatz
uspto-grants-1993_04
Patentnummer
US05200109

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