반응 #640547

반응 방정식

1,3-benzodioxole

sulfuryl chloride

→

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

수율 16.3%

용매

N,N-dimethylformamide

반응 조건

후처리

1. 1
   기타whereupon a solid formed
2. 2
   온도The reaction was cooled
3. 3
   추출extracted with methylene chloride
4. 4
   건조dried over magnesium sulfate
5. 5
   여과filtered
6. 6
   농축concentrated
7. 7
   기타to give 7.32 g of crude material as a black oil
8. 8
   기타This was chromatographed on silica gel using 20% methylene chloride/hexane

실험 절차

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.

출처