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Hydroxyethyl disulfide → 2-Methanesulfonyloxyethyl disulfide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydroxyethyl disulfide | HCID 15906 | — |
| 反応物 | Methanesulfonyl chloride | HCID 31297 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 2-Methanesulfonyloxyethyl disulfide | HCID 23117209 | — |
反応手順
N,N-Diisopropylethylamine (4.35 ml) and 1.70 ml of methanesulfonyl chloride were added to a suspension of 1.22 ml of 2-hydroxyethyl disulfide in 30 ml of dichloromethane at −40° C. under an argon atmosphere. The mixture was stirred at that temperature for 30 min. The reaction solution was then diluted with dichloromethane, and the diluted solution was washed with an dilute aqueous hydrochloric acid solution, an aqueous sodium hydrogencarbonate solution, and water in that order, and was dried over anhydrous magnesium sulfate. The solvent was removed by distillation under the reduced pressure to prepare 3.08 g of 2-methanesulfonyloxyethyl disulfide.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06680313B2 |
| 出典データセット | uspto-grants-2004_01 |
| ORD ID | ord-d13d244bb92a4400a4f1dbd341cc93ce |
| 出典メモ | uspto-grants-2004_01 |