Reaction #479219

Reaction equation

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

trioxane

→

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

Solvents

methanesulphonic acid

trifluoroacetic acid

Conditions

Workup

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

Procedure

0.37 g of 5-fluoro-benzo[b]thiophene-3-sulphonic acid-methylamide are dissolved in 5.9 ml of methanesulphonic acid at 35° C. and combined with a solution of 0.06 g of trioxane in 1.8 ml of trifluoroacetic acid. After 2.5 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: 0.22 g. M.p.: 175° C.

Source