1,3-Benzodioxole → 1,3-Benzodioxole-5-sulfonyl chloride
反応式
[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]1参加物
4
反応条件
- 温度
- 100 °C
実験手順
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.
後処理
- 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
出典と根拠
- ORDレコード
- ord-7c7f331849e741a384a746489950e6cd
- 出典データセット
- uspto-grants-2006_08
- 特許番号
- US07098202B2
反応ノート
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