Acetic Acid → 4-Fluoro-3-methylbenzohydrazide

HRID 239181Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 239181
C(O)(=O)C.C(OC([NH:12][NH:13][C:14](=[O:23])[C:15]1[CH:20]=[CH:19][C:18]([F:21])=[C:17]([CH3:22])[CH:16]=1)=O)(C)(C)C>ClCCl>[F:21][C:18]1[CH:19]=[CH:20][C:15]([C:14]([NH:13][NH2:12])=[O:23])=[CH:16][C:17]=1[CH3:22]

Komponenten

4

Edukt 2

HCID 176Acetic AcidHCID 86686514N'-(4-Fluoro-3-methyl-benzoyl)-hydrazinecarboxylic acid tert-butyl ester

Produkt 1

HCID 632093974-Fluoro-3-methylbenzohydrazideAusbeute 83,4 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

50 mL trifluor acetic acid was added to 13 g N′-(4-fluoro-3-methyl-benzoyl)-hydrazinecarboxylic acid tert-butyl ester in 150 mL dichlormethane. The reaction was stirred for 1 h at RT and the solvent was evaporated. The residue was basicfied with 1 N sodium hydroxide and extracted with saturated sodium chloride solution and tetrahydrofuran. The organic layer was evaporated and the residue crystallized from ethyl acetate to yield 6.8 g of the desired product.

Aufarbeitung

  1. customthe solvent was evaporated
  2. extractionextracted with saturated sodium chloride solution and tetrahydrofuran
  3. customThe organic layer was evaporated
  4. customthe residue crystallized from ethyl acetate

Quellen und Nachweise

ORD-Eintrag
ord-fba27b8f0c1c4370a96ed3d7253a19d1
Quelldatensatz
uspto-grants-2014_02
Patentnummer
US08642774B2

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