Water → HCID 53897658, Verbindung

HRID 620931Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 620931
[CH3:1][C:2]([NH:8][C:9](=[O:18])[C:10]1[CH:15]=[C:14]([Cl:16])[CH:13]=[C:12]([Cl:17])[CH:11]=1)([CH3:7])[C:3]([CH2:5]Cl)=[O:4].[C:19]([O-:22])(=[O:21])[CH3:20].[Na+].O>CN(C=O)C>[CH3:1][C:2]([NH:8][C:9](=[O:18])[C:10]1[CH:15]=[C:14]([Cl:16])[CH:13]=[C:12]([Cl:17])[CH:11]=1)([CH3:7])[C:3]([CH2:5][O:22][C:19](=[O:21])[CH3:20])=[O:4]

Komponenten

5

Edukt 3

HCID 962WaterHCID 517045Sodium AcetateHCID 54029353HCID 54029353, Verbindung

Produkt 1

HCID 53897658HCID 53897658, VerbindungAusbeute 47,4 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

N-(1',1'-dimethyl-3'-chloroacetonyl)-3,5-dichlorobenzamide (20 gm, 0.065 m) was dissolved in 100 ml of dry DMF and 10.6 gm (0.128 m) of sodium acetate was added. The slurry was blanketed under a nitrogen atmosphere and then heated to 80°-90° C. for 4 days. The reaction mixture was cooled by adding 100 ml of water. The aqueous solution was extracted four times with 10 ml aliquots of methylene chloride. The combined organic extracts were washed with water (3×100 ml) and brine. The solvent was removed, the resulting white solid dried and then recrystallized from an acetone and hexane (about 1:4) mixture to yield 10.2 gm of the product.

Aufarbeitung

  1. temperatureheated to 80°-90° C. for 4 days
  2. temperatureThe reaction mixture was cooled
  3. extractionThe aqueous solution was extracted four times with 10 ml aliquots of methylene chloride
  4. washThe combined organic extracts were washed with water (3×100 ml) and brine
  5. customThe solvent was removed
  6. customthe resulting white solid dried
  7. customrecrystallized from an acetone and hexane (about 1:4) mixture

Quellen und Nachweise

ORD-Eintrag
ord-4b3d8955cb444becb391239d267f1fe3
Quelldatensatz
uspto-grants-1989_04
Patentnummer
US04822902

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