2-Aminothiazole → HCID 14920282, Verbindung

HRID 918882Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 918882
CO[CH:3]=[C:4]([C:11]([O:13][CH3:14])=[O:12])[CH:5]=[CH:6][C:7]([O:9]C)=O.[NH2:15][C:16]1[S:17][CH:18]=[CH:19][N:20]=1>CN(C=O)C>[O:9]=[C:7]1[N:15]([C:16]2[S:17][CH:18]=[CH:19][N:20]=2)[CH:3]=[C:4]([C:11]([O:13][CH3:14])=[O:12])[CH:5]=[CH:6]1

Komponenten

4

Edukt 2

HCID 21552-AminothiazoleHCID 71338068Dimethyl 4-(methoxymethylidene)pent-2-enedioate

Produkt 1

HCID 14920282HCID 14920282, VerbindungAusbeute 43 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Reaktionsbedingungen

Temperatur
150 °C

Versuchsvorschrift

After 2 g (9.9 mmol) of dimethyl 4-(methoxymethylene)2-pentenedioate obtained in Example 1-1 was dissolved in 10 mL of DMF, 1 g (9.9 mmol) of 2-aminothiazole was added to the solution. Afterward, the resulting reaction solution was stirred under reflux at about 150° C. for 6 hours. After termination of the reaction was determined by liquid chromatography, the solvent was removed in vacuo and was then washed using brine, followed by drying using magnesium sulfate, and filtration. After distillation under reduced pressure, the resulting product was purified using column chromatography (hexane:ethylacetate=1:3) to obtain a target compound (Actual yield: 1 g, Percent yield: 43%).

Aufarbeitung

  1. customAfterward, the resulting reaction solution
  2. customthe solvent was removed in vacuo
  3. washwas then washed
  4. customby drying
  5. filtrationmagnesium sulfate, and filtration
  6. distillationAfter distillation under reduced pressure
  7. customthe resulting product was purified
  8. customto obtain a target compound (Actual yield: 1 g, Percent yield: 43%)

Quellen und Nachweise

ORD-Eintrag
ord-f38f9f6d475a4f5bae6ec4edbfe84b24
Quelldatensatz
uspto-grants-2016_03
Patentnummer
US09271976B2

Notizen zur Reaktion

Wird geladen…