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p-Toluenesulfonic acid → Triphenylsulfonium p-toluenesulfonate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | p-Toluenesulfonic acid | HCID 6101 | — |
| 反応物 | Triphenylsulfonium Bromide | HCID 11984010 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | Triphenylsulfonium p-toluenesulfonate | HCID 21872467 | 73.1% |
反応手順
A solution of triphenylsulfonium bromide (6.87 g, 20.0 mmol) and p-toluenesulfonic acid (3.80 g, 20.0 mmol) in water (100 ml) was heated at a gentle reflux for 15 hours under nitrogen. After cooling to room temperature, the clear solution was extracted with dichloromethane (4×75 ml). The combined organic extracts were washed with water until neutral (4×75 ml) and dried (MgSO4 ). The solvent was removed under reduced pressure and the residue dried by heating at 80° C. in vacuo for 36 hours to give a crude onium salt as a off-white solid (6.35 g). Recrystallization from acetone-ethyl acetate gave triphenylsulfonium rosylate as a white crystalline solid (5.72 g, 66%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05731364 |
| 出典データセット | uspto-grants-1998_03 |
| ORD ID | ord-859a3ba4fca04957adca8f06dc6bef2a |
| 出典メモ | uspto-grants-1998_03 |