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Pyridine → 2,2,3,3,3-Pentafluoropropyl p-Toluenesulfonate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Pyridine | HCID 1049 | — |
| 反応物 | 4-Toluenesulfonyl chloride | HCID 7397 | — |
| 反応物 | 2,2,3,3,3-Pentafluoropropanol | HCID 9872 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 溶媒 | Chloroform | HCID 6212 | — |
| 生成物 | 2,2,3,3,3-Pentafluoropropyl p-Toluenesulfonate | HCID 2776017 | 84% |
反応手順
To a solution of 2,2,3,3,3-pentafluoropropanol (5.0 mL, 50 mmol) and pyridine (8.1 mL, 100 mmol) in chloroform (100 mL), cooled at 0° C. and under argon, tosyl chloride (14.29 g, 75 mmol) was slowly added. The resulting mixture was allowed to warm up to room temperature and was stirred at this temperature overnight. Then, 10% aqueous K2CO3 solution was added and the mixture was vigorously stirred for 30 min. The layers were separated, and the organic layer was treated again with K2CO3. After that, it was washed with 2 N HCl, dried over Na2SO4 and the solvent was removed, yielding 12.72 g of the desired compound (84% yield).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07589125B2 |
| 出典データセット | uspto-grants-2009_09 |
| ORD ID | ord-cca5ac87c6764be8ab6a7016fb72dc67 |
| 出典メモ | uspto-grants-2009_09 |