化工社化工社 化学情報印刷レポート · 研究参考用
Dichloromethane → 4-(N-methylacetamido)benzene-1-sulfonyl chloride
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dichloromethane | HCID 6344 | — |
| 反応物 | N-Methylacetanilide | HCID 11364 | — |
| 反応物 | HCID 178527254 | HCID 178527254 | — |
| 生成物 | 4-(N-methylacetamido)benzene-1-sulfonyl chloride | HCID 293146 | 11% |
反応手順
A solution of N-methyl-N-phenylacetamide (11 g, 73.83 mmol) in dichloromethane (20 mL) was added dropwise to HSO3Cl (80 g, 689.66 mmol) at 5° C. The resulting solution was then stirred at room temperature overnight. The reaction mixture was then quenched by adding 100 mL of iced water. The resulting solution was extracted using dichloromethane (2×50 mL) and the organic layers were combined. The residue was purified by column chromatography using a 10:1 ethyl acetate/petroleum ether solvent system to give 2.2 g (11%) of 4-(N-methylacetamido)benzene-1-sulfonyl chloride as a white solid. 1H NMR (CDCl3) δ 8.09 (d, 2H), 7.48 (d, 2H), 3.38 (s, 3H), 2.17 (s, 3H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07696229B2 |
| 出典データセット | uspto-grants-2010_04 |
| ORD ID | ord-a751b95310f64630b0608d841bec1ac2 |
| 出典メモ | uspto-grants-2010_04 |