化工社化工社 化学情報印刷レポート · 研究参考用
Methanesulfonyl chloride → N-mesyl-O-(p-methoxybenzyl)hydroxylamine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methanesulfonyl chloride | HCID 31297 | — |
| 反応物 | O-((4-Methoxyphenyl)methyl)hydroxylamine | HCID 120426 | — |
| 溶媒 | Pyridine | HCID 1049 | — |
| 生成物 | N-mesyl-O-(p-methoxybenzyl)hydroxylamine | HCID 12763343 | 64.9% |
反応手順
63.0 g (0.55 mole) of mesyl chloride was added dropwise to a solution of 76.5 g (0.5 mole) of O-(p-methoxybenzyl)-hydroxylamine in 400 ml of pyridine while ice-cooling and stirring. After completion of the addition, the resulting mixture was stirred at room temperature (about 20°-30° C) for 5 hours and then the solvent was removed by distillation. 600 ml of ethyl acetate was added to the resulting residue, and the mixture was washed successively with 1N hydrochloric acid and water. The mixture was then dried and the solvent was distilled off to obtain 75 g (64.8% yield) of N-mesyl-O-(p-methoxybenzyl)hydroxylamine (IV) having a melting point of 114°-116° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04017512 |
| 出典データセット | uspto-grants-1977_04 |
| ORD ID | ord-663826d4311c464fab7daaf518a53796 |
| 出典メモ | uspto-grants-1977_04 |