関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2,3-Butanediol | HCID 262 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Methanesulfonyl chloride | HCID 31297 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 2,3-Butanediol, dimethanesulfonate | HCID 99909 | 98% |
反応手順
To a solution of butane 2,3-diol (15 g, 0.166 mol) and Et3N (57.7 mL, 0.415 mol) in CH2Cl2 (150 mL) at 0° C. was slowly added a solution of CH3SO2Cl (32.1 mL, 0.415 mol) in CH2Cl2 (75 mL). The mixture was stirred at 0° C. for 2 h and diluted with CH2Cl2. The mixture was washed with water, 1N HCl, 5% aqueous NaHCO3 and brine. The organic layer was dried over MgSO4, filtered and concentrated under reduced pressure to afford butane-2,3-diol dimethanesulfonate (40 g, 98%) as a light yellow oil. 1HNMR (CDCl3): δ 4.9 (m, 2H, CH), 3.05 (s, 6H, CH3), 1.4 (m, 6H, CH3).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08846972B2 |
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| 出典データセット | uspto-grants-2014_09 |
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| ORD ID | ord-0f3fd8bb40ac42499f2ea47afda727b8 |
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| 出典メモ | uspto-grants-2014_09 |
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