Реакция #8939

Уравнение реакции

1,3-benzodioxole

sulfuryl chloride

→

(1,3-benzodioxol-5-yl)sulfonyl chloride

Выход 16.3%

Растворители

N,N-dimethylformamide

Условия реакции

Обработка

1. 1
   Другоеwhereupon a solid formed
2. 2
   ТемператураThe reaction was cooled
3. 3
   Экстракцияextracted with methylene chloride
4. 4
   Сушкаdried over magnesium sulfate
5. 5
   Фильтрацияfiltered
6. 6
   Концентрированиеconcentrated
7. 7
   Другоеto give 7.32 g of crude material as a black oil
8. 8
   ДругоеThis was chromatographed on silica gel using 20% methylene chloride/hexane

Методика

To a solution of 4.25 g of anhydrous N,N-dimethylformamide at 0° C. under nitrogen was added 7.84 g of sulfuryl chloride, whereupon a solid formed. After stirring for 15 minutes, 6.45 g of 1,3-benzodioxole was added, and the mixture heated at 100° C. for 2 hours. The reaction was cooled, poured into ice water, extracted with methylene chloride, dried over magnesium sulfate, filtered and concentrated to give 7.32 g of crude material as a black oil. This was chromatographed on silica gel using 20% methylene chloride/hexane to afford 1.9 g of (1,3-benzodioxol-5-yl)sulfonyl chloride.

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