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Triethylamine → Tetrahydro-2H-pyran-3-ylmethyl 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 | Tetrahydro-2H-pyran-3-methanol | HCID 85769 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | Tetrahydro-2H-pyran-3-ylmethyl methanesulfonate | HCID 22402475 | — |
反応手順
To tetrahydro-2H-pyran-3-ylmethanol (4.92 g) in dry dichloromethane (140 ml) at 0° C. and under nitrogen, was added anhydrous triethylamine (13.6 ml) in one go, followed by mesyl chloride (4.3 ml) dropwise over 5 minutes. The reaction was allowed to warm to room temperature and stirred at this temperature overnight. The reaction was quenched with saturated aqueous sodium bicarbonate (50 ml). The organic layer was separated, passed through a hydrophobic frit to dry and concentrated in vacuo to yield a red oil (8.8 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07977344B2 |
| 出典データセット | uspto-grants-2011_07 |
| ORD ID | ord-da1ea2a94585412492498f6165dd4248 |
| 出典メモ | uspto-grants-2011_07 |