반응 #479217

반응 방정식

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

trioxane

→

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

용매

methanesulphonic acid

trifluoroacetic acid

반응 조건

후처리

1. 1
   기타The solid formed
2. 2
   기타is separated off by filtration
3. 3
   세척washed with 200 ml of water
4. 4
   workup.DISSOLUTIONdissolved while hot in 400 ml of ethanol/isopropanol (1:1)
5. 5
   기타separated from solid residues
6. 6
   여과by filtering again
7. 7
   기타is purified by chromatography

실험 절차

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.

출처