Reaktion #453501

Reaktionsgleichung

3-(2-carboxy-4-chloro-6-fluorobenzofuran-7-yl)-1-methyl-6-trifluoromethyluracil

→

desired product

Ausbeute 56.8%

3-(4-chloro-6-fluorobenzofuran-7-yl)-1-methyl-6-trifluoromethyluracil

Ausbeute 56.8%

Lösungsmittel

quinoline

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeAfter completion of the reaction
2. 2
   Filtrationthe reaction solution was subjected to filtration
3. 3
   ExtraktionThe filtrate was extracted with ethyl acetate
4. 4
   WaschenThe organic layer was washed sequentially with a 10% hydrochloric acid aqueous solution and water
5. 5
   Trocknendried over anhydrous sodium sulfate
6. 6
   workup.DISTILLATIONThe solvent was distilled off under reduced pressure
7. 7
   SonstigeThen, the obtained residue was purified by silica gel column chromatography

Vorschrift

7.0 g (17 mmol) of 3-(2-carboxy-4-chloro-6-fluorobenzofuran-7-yl)-1-methyl-6-trifluoromethyluracil and 5.0 g (79 mmol) of copper powder, were suspended in 50 ml of quinoline, followed by stirring at 200° C. for 1 hour. After completion of the reaction, the reaction solution was subjected to filtration. The filtrate was extracted with ethyl acetate. The organic layer was washed sequentially with a 10% hydrochloric acid aqueous solution and water and then dried over anhydrous sodium sulfate. The solvent was distilled off under reduced pressure. Then, the obtained residue was purified by silica gel column chromatography, to obtain 3.5 g (yield: 56%) of the desired product as white crystals. Melting point: 127-128° C.

Quelle