Réaction #479220

Équation de réaction

5-chloro-benzo[b]thiophene-3-sulphonic acid-methylamide

trioxane

→

6-chloro-4-methyl-4,5-dihydro-1,3-dithia-4-aza-acenaphthylene 3,3-dioxide

Solvants

methanesulphonic acid

trifluoroacetic acid

Conditions de réaction

Traitement

1. 1
   Extractionthe aqueous phase is extracted with ethyl acetate
2. 2
   SéchageThe combined organic extracts are dried with Na2SO4
3. 3
   Autreevaporated down in vacuo
4. 4
   Autrepurified by chromatography

Mode opératoire

0.60 g of 5-chloro-benzo[b]thiophene-3-sulphonic acid-methylamide are dissolved in 8.9 ml of methanesulphonic acid at 35° C. and combined with a solution of 0.09 g trioxane in 2.7 ml trifluoroacetic acid. After 3 h stirring at 35° C. the reaction mixture is poured onto 100 ml of ice water and the aqueous phase is extracted with ethyl acetate. The combined organic extracts are dried with Na2SO4, evaporated down in vacuo and then purified by chromatography. Yield: 0.30 g. M.p.: 196° C.

Source