Reaktion #483965

Reaktionsgleichung

NaOH

2,4-dibromoacetophenone

thioacetamide

→

title compound

Ausbeute 103.4%

4-(4-Bromophenyl)-2-methyl-1,3-thiazole

Ausbeute 103.4%

Lösungsmittel

dioxane

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturthe mixture was heated
2. 2
   Temperaturat reflux temperature for 8 hours
3. 3
   ExtraktionThe whole was extracted with diethyl ether
4. 4
   WaschenThe organic layer was washed with brine
5. 5
   Trocknendried over MgSO4
6. 6
   Einengenconcentrated in vacuo
7. 7
   SonstigeThe residue was purified by flash chromatography
8. 8
   Wascheneluting with ethyl acetate-hexane (1:5)

Vorschrift

To a stirred solution of 2,4-dibromoacetophenone (5 g, 18 mmol) in dioxane (180 ml) was added thioacetamide (6.76 g, 90 mmol), and the mixture was heated at reflux temperature for 8 hours. The reaction mixture was cooled down to room temperature, and made basic by addition of 2N NaOH aqueous solution. The whole was extracted with diethyl ether. The organic layer was washed with brine, dried over MgSO4, and concentrated in vacuo. The residue was purified by flash chromatography eluting with ethyl acetate-hexane (1:5) to give title compound (4.73 g, 99% yield).

Quelle