Reaktion #502814

Reaktionsgleichung

thioacetamide

2-bromo-1-(4-methoxy-phenyl)-ethanone

→

desired product

Ausbeute 69.6%

4-(4-Methoxy-phenyl)-2-methyl-thiazole

Ausbeute 69.6%

Lösungsmittel

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   Extraktionextracted with ethyl acetate (3×100 mL)
2. 2
   WaschenThe combined organics was washed with water, brine
3. 3
   Trocknendried (Na2SO4)
4. 4
   Filtrationfiltered
5. 5
   Einengenconcentrated
6. 6
   SonstigeThe crude residue was purified over silica gel (230-400 M, 1% EtOAc-Hexane)

Vorschrift

The mixture of thioacetamide (16.0 g, 213 mmol) and 2-bromo-1-(4-methoxy-phenyl)-ethanone (4.0 g, 17.5 mmol) was heated at 140° C. for 24 h under nitrogen atmosphere. After the completion of the reaction mixture (TLC monitoring), water (100 mL) was added and extracted with ethyl acetate (3×100 mL). The combined organics was washed with water, brine, dried (Na2SO4), filtered and concentrated. The crude residue was purified over silica gel (230-400 M, 1% EtOAc-Hexane) to get the desired product (2.5 g, 69%).

Quelle