Sodium Carbonate → HCID 10731614, Verbindung

HRID 580922

Reaktionsgleichung

Reaktionsgleichung von HRID 580922
[C:1]1([C:7]2[N:8]=[C:9]3[N:13]([CH:14]=2)[C:12]2[CH2:15][CH2:16][CH2:17][CH2:18][C:11]=2[S:10]3)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.P(Cl)(Cl)(Cl)=O.[C:24](=O)([O-])[O-:25].[Na+].[Na+]>CN(C)C=O>[C:1]1([C:7]2[N:8]=[C:9]3[N:13]([C:14]=2[CH:24]=[O:25])[C:12]2[CH2:15][CH2:16][CH2:17][CH2:18][C:11]=2[S:10]3)[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1

Komponenten

5

Edukt 3

HCID 10340Sodium CarbonateHCID 24813Phosphorus oxychlorideHCID 7608862-Phenyl-5,6,7,8-tetrahydroimidazo[2,1-b][1,3]benzothiazole

Produkt 1

HCID 10731614HCID 10731614, VerbindungAusbeute 82 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Reaktionsbedingungen

Temperatur
60 °C

Versuchsvorschrift

3.35 g of 5,6,7,8-tetrahydro-2-phenylimidazo[2,1-b]benzothiazole was suspended in 20 ml of dimethylformamide. To the resultant mixture, 3 ml of phosphorus oxychloride was added dropwise at 0° C. over 10 minutes. The solution was gradually returned to room temperature, then heated and stirred at 60° C. for 3 hours, poured onto an aqueous sodium carbonate solution, then extracted with chloroform. The solvent was distilled off, the residue was then recrystallized from ethanol to obtain the desired substance in an amount of 2.31 g (yield of 82.0%) (melting point:150-150.5° C.).

Aufarbeitung

  1. customwas gradually returned to room temperature
  2. temperatureheated
  3. extractionextracted with chloroform
  4. distillationThe solvent was distilled off
  5. customthe residue was then recrystallized from ethanol
  6. customto obtain the desired substance in an amount of 2.31 g (yield of 82.0%) (melting point:150-150.5° C.)

Quellen und Nachweise

ORD-Eintrag
ord-d1941fde172f477b96484c5054a58e59
Quelldatensatz
uspto-grants-1999_07
Patentnummer
US05919799

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