関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 2-Pyridinemethanamine | HCID 19509 | — |
| 反応物 | Methanesulfonyl chloride | HCID 31297 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | N-(pyridin-2-ylmethyl)methanesulfonamide | HCID 4657001 | 76.8% |
反応手順
To a 0° solution of 15 g of 2-(aminomethyl)pyridine, 15.44 g of triethylamine and 150 ml of methylene chloride is added 17.48 g of methanesulfonyl chloride in 100 ml of methylene chloride. The mixture is stirred at 0° C. for 1 hour followed by stirring at room temperature for 3 hours. The reaction is poured into saturated sodium bicarbonate and extracted with methylene chloride. The combined extracts are washed with saturated sodium chloride and concentrated in vacuo. The residue is purified by chromatography (silica gel: 10% methyl alcohol/ethyl acetate) to give 19.84 g of the desired product.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US05328921 |
|---|
| 出典データセット | uspto-grants-1994_07 |
|---|
| ORD ID | ord-ef97c1b6879e4165abc59e5e58371220 |
|---|
| 出典メモ | uspto-grants-1994_07 |
|---|