化工社化工社 化学情報印刷レポート · 研究参考用
Pyridine → Ethyl 2-methylsulfonyloxyethylcarbamate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Pyridine | HCID 1049 | — |
| 反応物 | Methanesulfonyl chloride | HCID 31297 | — |
| 反応物 | ethyl N-(2-hydroxyethyl)carbamate | HCID 223805 | — |
| 触媒 | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | Ethyl 2-methylsulfonyloxyethylcarbamate | HCID 19775872 | — |
反応手順
60 g of methanesulfonyl chloride are metered over approximately 30 minutes at 0° to +5° C. to a solution of 66.5 g of ethyl 2-hydroxyethylcarbamate, 43.5 g of pyridine and 1.9 g of 4-dimethylaminopyridine in 150 ml of methylene chloride, with stirring, and the mixture is stirred for 2 more hours at +5° C. and then for 16 hours at room temperature. The reaction mixture is filtered, the residue is washed with a small quantity of ethyl acetate, and the combined filtrates are washed with dilute hydrochloric acid and water. After the mixture has been dried over magnesium sulfate, the solvent mixture is removed completely by distillation in vacuo, which gives ethyl 2-methylsulfonyloxyethylcarbamate, nD20 1.4450.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05192803 |
| 出典データセット | uspto-grants-1993_03 |
| ORD ID | ord-d5c6d3b9d70e4c06980dc58cd703dd91 |
| 出典メモ | uspto-grants-1993_03 |