반응 #479220

반응 방정식

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

용매

methanesulphonic acid

trifluoroacetic acid

반응 조건

후처리

1. 1
   추출the aqueous phase is extracted with ethyl acetate
2. 2
   건조The combined organic extracts are dried with Na2SO4
3. 3
   기타evaporated down in vacuo
4. 4
   기타purified by chromatography

실험 절차

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.

출처