Ethanol → HCID 86743975, Verbindung

HRID 1651594Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1651594
Cl.[NH2:2][OH:3].[OH-:4].[Na+].O=[C:7]1[CH2:11][CH2:10][CH:9]([C:12]2[CH:21]=[C:20]3[C:15]([C:16](=[O:25])[CH:17]=[CH:18][N:19]3[CH:22]3[CH2:24][CH2:23]3)=[CH:14][C:13]=2[F:26])[CH2:8]1.[CH2:27]([OH:29])C>O>[N:2](=[C:7]1[CH2:11][CH2:10][CH:9]([C:12]2[CH:21]=[C:20]3[C:15]([C:16](=[O:25])[C:17]([C:27]([OH:29])=[O:4])=[CH:18][N:19]3[CH:22]3[CH2:24][CH2:23]3)=[CH:14][C:13]=2[F:26])[CH2:8]1)[OH:3]

Komponenten

6

Edukt 4

HCID 702EthanolHCID 14798Sodium Hydroxide2×HCID 443297Hydroxyamine hydrochlorideHCID 86743976HCID 86743976, Verbindung

Produkt 1

HCID 86743975HCID 86743975, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

A solution of 3.8 g (55 mol) of hydroxylamine hydrochloride in 100 ml of water was neutralized by the addition of 55 ml (55 mmol) of 1.0 N sodium hydroxide. To this was added a suspension of 16.5 g (50 mmol) of 7-(3-oxocyclopentyl)-1-cyclopropyl-6-fluoro-1,4-dihydro-4-oxoquinoline acid in a mixture of 150 ml of ethanol and 50 ml (50 mmol) of 1.0 N sodium hydroxide. The reaction mixture was heated at 60° for 4 hours and then at room temperature overnight. The alcohol was removed in vacuo and the aqueous was acidified to pH 2.0 with 6.0 M hydrochloric acid. The solid was removed by filtration, washed with water, and dried in vacuo to give 16.1 g of the title compound.

Aufarbeitung

  1. additionTo this was added
  2. temperatureThe reaction mixture was heated at 60° for 4 hours
  3. customat room temperature
  4. customovernight
  5. customThe alcohol was removed in vacuo
  6. customThe solid was removed by filtration
  7. washwashed with water
  8. customdried in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-7ad1ce2fbf104de9bf54a3d25f9dcfe0
Quelldatensatz
uspto-grants-1990_05
Patentnummer
US04929613

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