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Water → 2,2-Difluoropropane-1,3-diyl bis(4-methylbenzenesulfonate)
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | 4-Toluenesulfonyl chloride | HCID 7397 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 2,2-Difluoropropane-1,3-diol | HCID 95744 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 2,2-Difluoropropane-1,3-diyl bis(4-methylbenzenesulfonate) | HCID 44717450 | 71% |
反応手順
To a solution of 2,2-difluoropropane-1,3-diol (2.5 g, 22.3 mmol) in CH2Cl2 (100 mL) is added triethylamine (14.3 mL, 111.5 mmol) followed by 4-methyl-benzenesulfonyl chloride (12.8 g, 66.9 mmol). The reaction mixture is stirred for 16 h at room temperature. Water (35 mL) is added and the organic layer is separated and washed with more water (2×35 mL). The organic layer is concentrated and the crude compound is purified by flash column chromatography using EtOAc in heptane to afford the title compound (6.7 g, 71%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09150577B2 |
| 出典データセット | uspto-grants-2015_10 |
| ORD ID | ord-535cedb8697a4187928440bbe451479b |
| 出典メモ | uspto-grants-2015_10 |