Water → HCID 68587480, Verbindung

HRID 2070236Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2070236
[C:1]([C:5]1[CH:6]=[C:7]([OH:11])[CH:8]=[CH:9][CH:10]=1)([CH3:4])([CH3:3])[CH3:2].Cl[C:13]1[C:18]([C:19]([F:22])([F:21])[F:20])=[CH:17][C:16]([N+:23]([O-:25])=[O:24])=[C:15]([CH3:26])[CH:14]=1.C(=O)([O-])[O-].[K+].[K+].O>CN(C)C=O>[C:1]([C:5]1[CH:6]=[C:7]([CH:8]=[CH:9][CH:10]=1)[O:11][C:13]1[C:18]([C:19]([F:20])([F:22])[F:21])=[CH:17][C:16]([N+:23]([O-:25])=[O:24])=[C:15]([CH3:26])[CH:14]=1)([CH3:4])([CH3:2])[CH3:3]

Komponenten

6

Edukt 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 11450Phenol, 3-(1,1-dimethylethyl)-HCID 210179751-Chloro-5-methyl-4-nitro-2-(trifluoromethyl)benzene

Produkt 1

HCID 68587480HCID 68587480, VerbindungAusbeute 72 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

In 50 ml of N,N-dimethylformamide, 3.00 g (19.97 mmol) of 3-tertbutylphenol, 4.35 g (18.16 mmol) of 4-chloro-5-trifluoromethyl-2-methylnitrobenzene and 3.26 g (23.60 mmol) of potassium carbonate are heated at 50° C. for 15 min. The reaction solution is added to water and extracted repeatedly with dichloromethane, the extracts are dried over Na2SO4 and filtered and the solvent is removed under reduced pressure. The solid is washed with water and hexane and dried under reduced pressure. (6.6 g, purity 70.0%, yield 72.0%, log P (pH 2.3)=5.68).

Aufarbeitung

  1. extractionextracted repeatedly with dichloromethane
  2. dry with materialthe extracts are dried over Na2SO4
  3. filtrationfiltered
  4. customthe solvent is removed under reduced pressure
  5. washThe solid is washed with water and hexane
  6. customdried under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-51a2b8c425b44971bcf466b0d7d814bf
Quelldatensatz
uspto-grants-2012_10
Patentnummer
US08299301B2

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