Hydrochloric Acid → 4-Bromo-5-fluoro-2-hydrazinylbenzoic acid hydrochloride

HRID 523234

Reaktionsgleichung

[Br:1][C:2]1[C:10]([F:11])=[CH:9][C:5]([C:6]([OH:8])=[O:7])=[C:4](F)[CH:3]=1.[NH2:13][NH2:14].[ClH:15]>CN1CCCC1=O>[ClH:15].[Br:1][C:2]1[C:10]([F:11])=[CH:9][C:5]([C:6]([OH:8])=[O:7])=[C:4]([NH:13][NH2:14])[CH:3]=1

Komponenten

Reaktionsbedingungen

Temperatur: 95 °C

Versuchsvorschrift

A mixture of 4-bromo-2,5-difluorobenzoic acid (2.50 g, 10.6 mmol) and hydrazine (3.81 mL, 121 mmol) in N-methyl-2-pyrrolidinone (2 mL) was heated at 95° C. for 4 h. The cooled mixture was poured into vigorously stirred 6 M aqueous HCl (400 mL) which was cooled in an NaCl-ice bath. The resulting precipitate was collected by filtration, washed with 6 M aqueous HCl (200 mL) and dried under vacuum to give 4-bromo-5-fluoro-2-hydrazinylbenzoic acid hydrochloride as a yellow solid (1.88 g, 71% purity, 44% yield), used without further purification.

Aufarbeitung

temperaturewas cooled in an NaCl-ice bath
filtrationThe resulting precipitate was collected by filtration
washwashed with 6 M aqueous HCl (200 mL)
customdried under vacuum

Quellen und Nachweise

ORD-Eintrag: ord-7d586237e60148f69ccfc0d9b881c500
Quelldatensatz: uspto-grants-2016_05
DOI: 10.6084/m9.figshare.5104873.v1
Patentnummer: US09334290B2

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