関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Methanesulfonyl chloride | HCID 31297 | — |
| 反応物 | Tetrahydro-3-furanmethanol | HCID 139980 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | Methanesulfonate | HCID 85257 | — |
| 生成物 | Tetrahydro-3-furanmethanol | HCID 139980 | — |
反応手順
Triethylamine (13.7 mL, 98 mmol) was added to a solution of tetrahydro-3-furanmethanol (10.0 g, 98 mmol) in methylene chloride (100 mL) at 0° C. followed by addition of methanesulfonyl chloride (12.3 g, 108 mmol) dropwise. The reaction mixture was stirred at 0° C. for 1 h and then allowed to warm to ambient temperature and stirred overnight. Aqueous hydrochloric acid (1N, 100 mL) was added and the two layers were separated. The organic layer was washed with 1N aqueous hydrochloric acid (100 mL×2), saturated aqueous sodium bicarbonate (100 mL×3), and brine (50 mL×1), respectively. The organic phase was dried over anhydrous sodium sulfate and concentrated to afford crude mesylate of tetrahydro-3-furanmethanol.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09434761B2 |
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| 出典データセット | uspto-grants-2016_09 |
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| ORD ID | ord-75b92de63ae14e078729bd2eb9210720 |
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| 出典メモ | uspto-grants-2016_09 |
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