Reaktion #344314

Reaktionsgleichung

7-hydroxymethylbenzo-1,2,3-thiadiazole

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title compound

Ausbeute 91.5%

benzo-1,2,3-thiadiazole-7-carbaldehyde

Ausbeute 91.5%

Lösungsmittel

chloroform

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigerises briefly to 31° C
2. 2
   workup.ADDITIONWhen the temperature has dropped again to 25° C.
3. 3
   Temperaturthe mixture is heated
4. 4
   Temperaturrefluxed overnight
5. 5
   Temperaturheating of the mixture
6. 6
   FiltrationThe hot mixture is filtered over Hyflo
7. 7
   Sonstigethe filtrate is then evaporated
8. 8
   Filtrationfiltered

Vorschrift

To a solution of 16.6 g of 7-hydroxymethylbenzo-1,2,3-thiadiazole in 100 ml of chloroform there are introduced with stirring at room temperature 35 g of manganese dioxide, during which process the internal temperature rises briefly to 31° C. When the temperature has dropped again to 25° C., the mixture is heated and refluxed overnight. Another 5 g of manganese dioxide are subsequently added, and heating of the mixture is continued until the reaction is complete. The hot mixture is filtered over Hyflo and the filtrate is then evaporated. The residue is digested in a little hexane and then filtered, which gives 15 g (91.4%) of the title compound of m.p. 134°-136° C.

Quelle