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Tetraethylene Glycol → 1,11-Bis(methanesulfonyloxy)-3,6,9-trioxandecane
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Tetraethylene Glycol | HCID 8200 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Methanesulfonyl chloride | HCID 31297 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 1,11-Bis(methanesulfonyloxy)-3,6,9-trioxandecane | HCID 3637875 | 99.8% |
反応手順
15 g of tetraethyleneglycol and 23.4 g of triethylamine were dissolved in 200 mL of dichloromethane, to which 22.1 g of methanesulfonylchloride was added dropwise at 0° C., and then the solution was stirred for 1 hour. The reaction solution was filtrated to remove insolubles, and then the filtrate was concentrated under reduced pressure. The residue was separated with ethyl acetate-water, and the organic layer was concentrated under reduced pressure after washing with water. The residue was purified with silica gel column chromatography to obtain 27 g of the objective compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07655768B2 |
| 出典データセット | uspto-grants-2010_02 |
| ORD ID | ord-9c055947ea344fc89bbc27ee17e3b262 |
| 出典メモ | uspto-grants-2010_02 |