2-Chloro-3',4'-dihydroxyacetophenone → HCID 178515889, Verbindung

HRID 483361

Reaktionsgleichung

Reaktionsgleichung von HRID 483361
Cl[CH2:2][C:3]([C:5]1[CH:10]=[CH:9][C:8]([OH:11])=[C:7]([OH:12])[CH:6]=1)=O.[C:13](=[S:16])([S-:15])[NH2:14].[NH4+]>CO>[OH:12][C:7]1[CH:6]=[C:5]([C:3]2[N:14]=[C:13]([SH:16])[S:15][CH:2]=2)[CH:10]=[CH:9][C:8]=1[OH:11]

Komponenten

4

Edukt 2

HCID 668342-Chloro-3',4'-dihydroxyacetophenoneHCID 11083854Ammonium dithiocarbamate

Produkt 1

HCID 178515889HCID 178515889, VerbindungAusbeute 72,9 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

10.0 g (53.6 mmol) of 2-chloro-3'4'-dihydroxyacetophenone was dissolved in 100 ml of methanol, and then 5.90 g (53.6 mmol) of ammonium dithiocarbamate was added thereto. The mixture was stirred at room temperature for 30 minutes. The solvent was distilled off under reduced pressure. To the residue, water was added to adjust the mixture to pH2.0, and then the mixture was extracted twice with ethyl acetate. The extract was dried over anhydrous sodium sulfate and-then concentrated. The crystal residue was washed with diethyl ether to obtain 8.80 g (yield: 72.9%) of the above-identified compound.

Aufarbeitung

  1. distillationThe solvent was distilled off under reduced pressure
  2. additionTo the residue, water was added
  3. extractionthe mixture was extracted twice with ethyl acetate
  4. dry with materialThe extract was dried over anhydrous sodium sulfate
  5. concentrationconcentrated
  6. washThe crystal residue was washed with diethyl ether

Quellen und Nachweise

ORD-Eintrag
ord-2415b5230c51422e806ffa8b944759b4
Quelldatensatz
uspto-grants-1993_07
Patentnummer
US05225406

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