Реакция #479220

Уравнение реакции

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

Растворители

methanesulphonic acid

trifluoroacetic acid

Условия реакции

Обработка

1. 1
   Экстракцияthe aqueous phase is extracted with ethyl acetate
2. 2
   СушкаThe combined organic extracts are dried with Na2SO4
3. 3
   Другоеevaporated down in vacuo
4. 4
   Другоеpurified by chromatography

Методика

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.

Источник