Potassium Carbonate → HCID 18966674, Verbindung

HRID 2226192

Reaktionsgleichung

Reaktionsgleichung von HRID 2226192
[Cl:1][C:2]1[CH:7]=[C:6]([O:8][C:9]2[CH:14]=[CH:13][CH:12]=[C:11]([C:15]([F:18])([F:17])[F:16])[CH:10]=2)[CH:5]=[CH:4][C:3]=1[OH:19].Cl[CH2:21][CH2:22][NH:23][C:24](=[O:28])[O:25][CH2:26][CH3:27].C(=O)([O-])[O-].[K+].[K+]>>[Cl:1][C:2]1[CH:7]=[C:6]([O:8][C:9]2[CH:14]=[CH:13][CH:12]=[C:11]([C:15]([F:17])([F:18])[F:16])[CH:10]=2)[CH:5]=[CH:4][C:3]=1[O:19][CH2:21][CH2:22][NH:23][C:24](=[O:28])[O:25][CH2:26][CH3:27]

Komponenten

4

Edukt 3

HCID 11430Potassium CarbonateHCID 80621Ethyl 2-chloroethylcarbamateHCID 189667272-Chloro-4-(3-trifluoromethylphenoxy)phenol

Produkt 1

HCID 18966674HCID 18966674, Verbindung

Versuchsvorschrift

To a solution of 0.5 g (1.73 mmol) of 2-chloro-4-(3-trifluoromethylphenoxy)phenol in 20 ml of N,N-dimethylfomamide, there are added 0.29 g (1.90 mmol) of ethyl 2-chloroethylcarbamate and 0.53 g (3.81 mmol) of potassium carbonate with stirring, and the resultant mixture is heated at 50° C. for 7 hours. The reaction mixture is poured into 100 g of ice-water and extracted twice with 100 ml of ethyl acetate. The extracts are combined together, dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The residue is subjected to silica gel chromatography to give ethyl 2-[2-chloro-4-(3-trifluoromethylphenoxy)phenoxy]ethylcarbamate.

Aufarbeitung

  1. extractionextracted twice with 100 ml of ethyl acetate
  2. dry with materialdried over anhydrous magnesium sulfate
  3. concentrationconcentrated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-8556cf1b172d4d51aa2ee21f73a61735
Quelldatensatz
uspto-grants-1994_09
Patentnummer
US05346920

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