Réaction #479217

Équation de réaction

N-ethyl-benzo[b]thiophene-3-sulphonamide

trioxane

→

4-ethyl-4,5-dihydro-1,3-dithia-4-aza-acenaphthylene 3,3-dioxide

Solvants

methanesulphonic acid

trifluoroacetic acid

Conditions de réaction

Traitement

1. 1
   AutreThe solid formed
2. 2
   Autreis separated off by filtration
3. 3
   Lavagewashed with 200 ml of water
4. 4
   workup.DISSOLUTIONdissolved while hot in 400 ml of ethanol/isopropanol (1:1)
5. 5
   Autreseparated from solid residues
6. 6
   Filtrationby filtering again
7. 7
   Autreis purified by chromatography

Mode opératoire

1.90 g of N-ethyl-benzo[b]thiophene-3-sulphonamide are dissolved in 25 ml methanesulphonic acid at 35° C. and combined with a solution of 0.29 g of trioxane in 8 ml of trifluoroacetic acid. After 2.5 h stirring at ambient temperature the reaction mixture is poured onto 400 ml of ice water. The solid formed is separated off by filtration, washed with 200 ml of water and then dissolved while hot in 400 ml of ethanol/isopropanol (1:1) and separated from solid residues by filtering again. The residue remaining after the concentration of the filtrate is purified by chromatography. Yield: 0.82 g. M.p.: 156° C.

Source