関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 1,3-Benzodioxole | HCID 9229 | — |
| 反応物 | Sulfuryl chloride | HCID 24648 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 1,3-Benzodioxole-5-sulfonyl chloride | HCID 4913401 | 16.3% |
反応手順
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.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07098202B2 |
|---|
| 出典データセット | uspto-grants-2006_08 |
|---|
| ORD ID | ord-7c7f331849e741a384a746489950e6cd |
|---|
| 出典メモ | uspto-grants-2006_08 |
|---|