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Triethylamine → Hex-5-yn-1-yl methanesulfonate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Methanesulfonyl chloride | HCID 31297 | — |
| 反応物 | 5-Hexyn-1-ol | HCID 70234 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | Hex-5-yn-1-yl methanesulfonate | HCID 12714590 | — |
反応手順
A solution of methanesulphonyl chloride (23.7 ml) in dry dichloromethane (25 ml.) was added dropwise to a solution of hex-5-yn-1-ol (Lancaster Synthesis, 25 g) and triethylamine (47.3 ml) in dichloromethane (300 ml), stirred under a nitrogen atmosphere at -70°. The resulting mixture was allowed to warm to room temperature over 16 hours. The mixture was then washed with water, dilute hydrochloric acid, saturated sodium bicarbonate solution and brine before drying over anhydrous magnesium sulphate and evaporation in vacuo. Hex-5-ynyl methanesulphonate was obtained as an oil (43.6 g) and was used without purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05466710 |
| 出典データセット | uspto-grants-1995_11 |
| ORD ID | ord-f34665ecde3e4391abcf6b27dc244d0d |
| 出典メモ | uspto-grants-1995_11 |