Water → HCID 53897658, Verbindung

HRID 342752Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 342752
[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-f19ab130800a4b1d90ff51182f3c0aed
Quelldatensatz
uspto-grants-1999_01
Patentnummer
US05859063

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