Sodium Bicarbonate → HCID 85787172, Verbindung

HRID 1865383Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1865383
Br[CH:2]([C:9](=[O:14])[C:10]([CH3:13])([CH3:12])[CH3:11])[C:3](=O)[C:4]([CH3:7])([CH3:6])[CH3:5].[NH2:15][C:16]([NH2:18])=[S:17].C(=O)([O-])O.[Na+]>C(O)C>[NH2:18][C:16]1[S:17][C:2]([C:9](=[O:14])[C:10]([CH3:13])([CH3:12])[CH3:11])=[C:3]([C:4]([CH3:7])([CH3:6])[CH3:5])[N:15]=1

Komponenten

5

Edukt 3

HCID 516892Sodium BicarbonateHCID 546382Bromo-dipivaloylmethaneHCID 2723790Thiourea

Produkt 1

HCID 85787172HCID 85787172, VerbindungAusbeute 94,8 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

A mixture of 4-bromo-2,2,6,6-tetramethyl-3,5-heptanedione (α-bromo-dipivaloylmethane; 1.42 g, 5.40 mmol), thiourea(451.8 mg, 5.94 mmol) and ethanol(15 mL) was refluxed for 2 hours. After the reaction mixture was cooled to room temperature, it was poured into saturated aqueous sodium hydrogen carbonate and extracted with ethyl acetate. After the ethyl acetate layer was washed successively with water and brine, dried over anhydrous sodium sulfate, the residue obtained by evaporation of the solvent under reduced pressure was crystallized by dichloromethane/n-hexane to give the title compound(1.23 g, 94.5%) as a white crystal.

Aufarbeitung

  1. temperaturewas refluxed for 2 hours
  2. extractionextracted with ethyl acetate
  3. washAfter the ethyl acetate layer was washed successively with water and brine
  4. dry with materialdried over anhydrous sodium sulfate
  5. customthe residue obtained by evaporation of the solvent under reduced pressure
  6. customwas crystallized by dichloromethane/n-hexane

Quellen und Nachweise

ORD-Eintrag
ord-25a823ac4892465284d53ac0aeadec24
Quelldatensatz
uspto-grants-2009_12
Patentnummer
US07626042B2

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