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Water → HCID 66939361, Verbindung

HRID 1257422
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1257422
[OH:1][N:2]=[C:3]([C:5]1[CH:10]=[CH:9][CH:8]=[C:7]([C:11]([F:14])([F:13])[F:12])[CH:6]=1)[NH2:4].Cl[C:16](=O)[CH2:17][N:18]1[CH:22]=[C:21]([C:23]([O:25][CH2:26][CH3:27])=[O:24])[CH:20]=[N:19]1.O>N1C=CC=CC=1>[F:14][C:11]([F:13])([F:12])[C:7]1[CH:6]=[C:5]([C:3]2[N:4]=[C:16]([CH2:17][N:18]3[CH:22]=[C:21]([C:23]([O:25][CH2:26][CH3:27])=[O:24])[CH:20]=[N:19]3)[O:1][N:2]=2)[CH:10]=[CH:9][CH:8]=1
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 962WaterHCID 609330N'-hydroxy-3-(trifluoromethyl)benzimidamideHCID 58127969HCID 58127969, Verbindung

Produkt 1

HCID 66939361HCID 66939361, VerbindungAusbeute 10,1 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1049PyridineLösungsmittel

Reaktionsbedingungen

Temperatur
115 °C

Versuchsvorschrift

A solution of N′-hydroxy-3-(trifluoromethyl)benzenecarboximidamide (2.1 g) in pyridine (20 mL) was cooled in an ice bath, and the compound (2.3 g) obtained in Example 115c was added. The reaction mixture was stirred overnight with heating at 110-120° C. The mixture was poured into water, and the mixture was extracted with ethyl acetate. The ethyl acetate layer was separated, washed successively with 1N hydrochloric acid and saturated brine, dried over sodium sulfate, and concentrated under reduced pressure. The residue was purified by column chromatography (carrier: silica gel, eluent: petroleum ether-ethyl acetate) to give the title compound (0.38 g) as a solid.

Aufarbeitung

  1. extractionthe mixture was extracted with ethyl acetate
  2. customThe ethyl acetate layer was separated
  3. washwashed successively with 1N hydrochloric acid and saturated brine
  4. dry with materialdried over sodium sulfate
  5. concentrationconcentrated under reduced pressure
  6. customThe residue was purified by column chromatography (carrier: silica gel, eluent: petroleum ether-ethyl acetate)

Quellen und Nachweise

ORD-Eintrag
ord-bbb7264266f546f2b8552eebeb0808ec
Quelldatensatz
uspto-grants-2013_06
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08461348B2

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