Reaktion #453499

Reaktionsgleichung

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

sulfuric acid

→

desired product

Ausbeute 88.4%

3-(4-chloro-6-fluoro-2-formylbenzofuran-7-yl)-1-methyl-6-trifluoromethyluracil

Ausbeute 88.4%

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeAfter completion of the reaction
2. 2
   Extraktionextracted with ethyl acetate
3. 3
   WaschenThe organic layer was washed sequentially with a saturated sodium hydrogencarbonate aqueous solution, water
4. 4
   Trocknena saturated sodium chloride aqueous solution, and then dried over anhydrous sodium sulfate
5. 5
   workup.DISTILLATIONThe solvent was distilled off under reduced pressure
6. 6
   SonstigeThen, the obtained residue was crystallized from isopropyl ether

Vorschrift

60 ml of concentrated sulfuric acid was added to 12.0 g (22.5 mmol) of 3-(4-chloro-2-dibromomethyl-6-fluorobenzofuran-7-yl)-1-methyl-6-trifluoromethyluracil, followed by stirring at 50° C. for 1 hour. After completion of the reaction, the reaction solution was poured into ice water and extracted with ethyl acetate. The organic layer was washed sequentially with a saturated sodium hydrogencarbonate aqueous solution, water and a saturated sodium chloride aqueous solution, and then dried over anhydrous sodium sulfate. The solvent was distilled off under reduced pressure. Then, the obtained residue was crystallized from isopropyl ether to obtain 7.6 g (yield: 88.4%) of the desired product as pale yellow crystals. Melting point: 180-183° C.

Quelle