Hydroxyamine hydrochloride → (NZ)-N-[(4-chloro-2-fluoro-5-methoxyphenyl)-[4-(4-chlorophenoxy)-2-propylphenyl]methylidene]hydroxylamine

HRID 1172827Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1172827
[Cl:1][C:2]1[CH:29]=[CH:28][C:5]([O:6][C:7]2[CH:12]=[CH:11][C:10]([C:13]([C:15]3[CH:20]=[C:19]([O:21][CH3:22])[C:18]([Cl:23])=[CH:17][C:16]=3[F:24])=O)=[C:9]([CH2:25][CH2:26][CH3:27])[CH:8]=2)=[CH:4][CH:3]=1.Cl.[NH2:31][OH:32].C([O-])(=O)C.[Na+]>C(O)C>[Cl:1][C:2]1[CH:29]=[CH:28][C:5]([O:6][C:7]2[CH:12]=[CH:11][C:10](/[C:13](/[C:15]3[CH:20]=[C:19]([O:21][CH3:22])[C:18]([Cl:23])=[CH:17][C:16]=3[F:24])=[N:31]/[OH:32])=[C:9]([CH2:25][CH2:26][CH3:27])[CH:8]=2)=[CH:4][CH:3]=1

Komponenten

5

Edukt 3

HCID 443297Hydroxyamine hydrochlorideHCID 517045Sodium AcetateHCID 68689947[4-(4-Chlorophenoxy)-2-propylphenyl][4-chloro-2-fluoro-5-methoxyphenyl]methanone

Produkt 1

HCID 87541464(NZ)-N-[(4-chloro-2-fluoro-5-methoxyphenyl)-[4-(4-chlorophenoxy)-2-propylphenyl]methylidene]hydroxylamine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Reaktionsbedingungen

Temperatur
60 °C

Versuchsvorschrift

A mixture of the product from Step 3 (1.4 g, 3.2 mmol), hydroxylamine hydrochloride (2.2 g, 32 mmol) and sodium acetate (2.6 g, 32 mmol) in ethanol (30 mL) was stirred in a sealed tube at 60° C. for 72 h. The precipitate was filtered off and the filtrate was concentrated. The residue was purified by chromatography on silica gel to give the oxime product.

Aufarbeitung

  1. filtrationThe precipitate was filtered off
  2. concentrationthe filtrate was concentrated
  3. customThe residue was purified by chromatography on silica gel

Quellen und Nachweise

ORD-Eintrag
ord-03cfe079c7e142128b5e3fbbf56af84c
Quelldatensatz
uspto-grants-2010_11
Patentnummer
US07834036B2

Notizen zur Reaktion

Wird geladen…