化工社化工社 化学情報印刷レポート · 研究参考用
Chloroform → 2,4-Difluoro-5-methylbenzenesulfonyl chloride
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Chloroform | HCID 6212 | — |
| 反応物 | Chlorosulfonic acid | HCID 24638 | — |
| 反応物 | 2,4-Difluoro-1-methylbenzene | HCID 67983 | — |
| 生成物 | 2,4-Difluoro-5-methylbenzenesulfonyl chloride | HCID 59436530 | 75.1% |
反応手順
Chlorosulfonic acid (5.2 mL, 0.078 mol) was added dropwise to a solution of 2,4-difluorotoluene (4.00 g, 0.0312 mol) in chloroform (75 mL, 0.94 mol). The reaction was stirred 2 hours. Additional chlorosulfonic acid (3.1 mL, 0.047 mol) was added and stirring was continued for 18 hours. The reaction was evaporated to an oil and poured onto ice. The mixture was extracted two times with ethyl ether. The combined organic phase was dried over magnesium sulfate and treated with activated carbon. The mixture was filtered through diatomaceous earth and the filtrate was evaporated to give 5.31 g of light brown oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08541588B2 |
| 出典データセット | uspto-grants-2013_09 |
| ORD ID | ord-6a7202be207d4465aeb64585adedb843 |
| 出典メモ | uspto-grants-2013_09 |