Ammonium Acetate → HCID 178517437, Verbindung

HRID 1414509Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1414509
ClC(Cl)(Cl)[C:3]([NH:5][C:6]1[S:7][CH:8]=[CH:9][C:10]=1[C:11](=O)[C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1)=[O:4].C([O-])(=O)C.[NH4+:25]>CS(C)=O>[C:12]1([C:11]2[C:10]3[CH:9]=[CH:8][S:7][C:6]=3[NH:5][C:3](=[O:4])[N:25]=2)[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1

Komponenten

4

Edukt 2

HCID 517165Ammonium AcetateHCID 214877322-Trichloroacetamido-3-benzoylthiophene

Produkt 1

HCID 178517437HCID 178517437, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 679Dimethyl SulfoxideLösungsmittel

Reaktionsbedingungen

Temperatur
95 °C

Versuchsvorschrift

To a solution of 2.0 g of 2-trichloroacetamido-3-benzoylthiophene in 18 ml of dimethylsulfoxide was added 0.89 g of ammonium acetate. The mixture was heated at 95° C for 2 hours, and poured into ice water, and extracted with chloroform. The chloroform layer was washed with water, dried over sodium sulfate, and the solvent was removed under reduced pressure. The residue was chromatographed on 60 g of silica gel, using methanol as an eluent to obtain 4-phenyl-1,2-dihydrothieno(2,3-d)-pyrimidin-2-one as crystals. Recrystallized from chloroform-acetone, the crystals having a melting point of 247.5°- 249° C. were obtained.

Aufarbeitung

  1. extractionextracted with chloroform
  2. washThe chloroform layer was washed with water
  3. dry with materialdried over sodium sulfate
  4. customthe solvent was removed under reduced pressure
  5. customThe residue was chromatographed on 60 g of silica gel

Quellen und Nachweise

ORD-Eintrag
ord-dd6ea2bd164142d98a44efb1ba70d899
Quelldatensatz
uspto-grants-1977_01
Patentnummer
US04001412

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