1,3-Benzodioxole → 1,3-Benzodioxole-5-sulfonyl chloride
반응식
[S:1]([Cl:5])(Cl)(=[O:3])=[O:2].[O:6]1[C:10]2[CH:11]=[CH:12][CH:13]=[CH:14][C:9]=2[O:8][CH2:7]1>CN(C)C=O>[O:6]1[C:10]2[CH:11]=[CH:12][C:13]([S:1]([Cl:5])(=[O:3])=[O:2])=[CH:14][C:9]=2[O:8][CH2:7]1참가 물질
4
반응 조건
- 온도
- 100 °C
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.
후처리
- customwhereupon a solid formed
- temperatureThe reaction was cooled
- extractionextracted with methylene chloride
- dry with materialdried over magnesium sulfate
- filtrationfiltered
- concentrationconcentrated
- customto give 7.32 g of crude material as a black oil
- customThis was chromatographed on silica gel using 20% methylene chloride/hexane
출처 및 근거
- ORD 기록
- ord-771a37b166694f87a54ba1bf13c55b3c
- 출처 데이터셋
- uspto-grants-2006_08
- 특허 번호
- US07091219B2
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