Reaktion #62040

Reaktionsgleichung

2-Cyano-2-[4-(2,5-dichloro-phenoxy)-3-fluoro-phenylthiocarbamoyl]-acetamide

bromine

→

5-[4-(2,5-Dichloro-phenoxy)-3-fluoro-phenylamino]-3-hydroxy-isothiazole-4-carbonitrile

Lösungsmittel

ethyl acetate

ethyl acetate

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONAfter addition
2. 2
   workup.STIRRINGthe reaction mixture was stirred for another 3 hours
3. 3
   FiltrationThe precipitate was filtered
4. 4
   Waschenthe solid was washed with ethyl ether
5. 5
   workup.STIRRINGwith stirring for 10 min
6. 6
   FiltrationThe solid was filtered
7. 7
   Waschenwashed with water
8. 8
   Sonstigedried in vacuo
9. 9
   Sonstigeto afford a white powder

Vorschrift

2-Cyano-2-[4-(2,5-dichloro-phenoxy)-3-fluoro-phenylthiocarbamoyl]-acetamide (1.6 g, 4 mmol) was dissolved in anhydrous ethyl acetate (60 ml) and a solution of bromine (0.2 ml, 4 mmol) in anhydrous ethyl acetate (10 ml) was added dropwise into the mixture with stirring at room temperature. After addition, the reaction mixture was stirred for another 3 hours. The precipitate was filtered and the solid was washed with ethyl ether and suspended in a saturated sodium bicarbonate with stirring for 10 min. The solid was filtered, then washed with water and dried in vacuo to afford a white powder.

Quelle