Reaktion #344324

Reaktionsgleichung

7-(1,1,1-trichloro-2-hydroxyeth-2-yl)benzo-1,2,3-thiadiazole

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title compound

7-trichloroacetylbenzo-1,2,3-thiadiazole

Lösungsmittel

chloroform

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturrefluxed for 16 hours
2. 2
   TemperaturAfter a total of 40 hours, the mixture is cooled
3. 3
   Filtrationfiltered twice through Hyflo
4. 4
   Sonstigethe filtrate is evaporated
5. 5
   Sonstigepurified

Vorschrift

A solution of 2.8 g of 7-(1,1,1-trichloro-2-hydroxyeth-2-yl)benzo-1,2,3-thiadiazole in 30 ml of chloroform is treated with 5 g of manganese dioxide and refluxed for 16 hours, with stirring. A further 5 and 3 g of manganese dioxide are added at intervals of 16 hours and 8 hours, respectively. After a total of 40 hours, the mixture is cooled and filtered twice through Hyflo, the filtrate is evaporated and purified using silica gel (hexane/ethyl acetate 7:3), giving the title compound of refractive index nD26 =1.6178.

Quelle