化工社化工社 化学情報印刷レポート · 研究参考用
m-Chloroperbenzoic acid → N-(2-Chloro-6-methanesulfonylmethyl-phenyl)-2,2,2-trifluoro-acetamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | m-Chloroperbenzoic acid | HCID 70297 | — |
| 反応物 | Alumina | HCID 9989226 | — |
| 反応物 | N-(2-Chloro-6-methylsulfanylmethyl-phenyl)-2,2,2-trifluoro-acetamide | HCID 22574009 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | N-(2-Chloro-6-methanesulfonylmethyl-phenyl)-2,2,2-trifluoro-acetamide | HCID 22574080 | — |
反応手順
The crude solid N-(2-chloro-6-methylsulfanylmethyl-phenyl)-2,2,2-trifluoro-acetamide from Step 2 was redissolved in methylene chloride (300 ml) and treated at 0° C. with meta-chloroperoxybenzoic acid (39.88 g, 0.177 mole) in portions with stirring. After 90 minutes the entire reaction mixture was poured onto a column of deactivated aluminum oxide (6% water) and the product was washed free of the acid by eluting with 1:1 ethyl acetate:hexane to afford 22.28 g of N-(2-Chloro-6-methanesulfonylmethyl-phenyl)-2,2,2-trifluoro-acetamide, a crystalline product (86%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06852726B2 |
| 出典データセット | uspto-grants-2005_02 |
| ORD ID | ord-52c4651d64e1430795428fe882f2b19a |
| 出典メモ | uspto-grants-2005_02 |