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Sodium Iodide → Dimesityl disulfide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Iodide | HCID 5238 | — |
| 反応物 | 2-Mesitylenesulfonyl chloride | HCID 13046 | — |
| 反応物 | Acetic acid, 2-fluoro-, 1,1'-anhydride | HCID 67886 | — |
| 溶媒 | Acetone | HCID 180 | — |
| 生成物 | Dimesityl disulfide | HCID 345613 | — |
反応手順
2,4,6-trimethylphenylsulfonyl chloride (500 mg, 2.3 mmol) was dissolved in acetone (60 mL), and then NaI (3.4 g, 23 mmol) and fluoroacetic anhydride (1.45 mL, 6.9 mmol) were added and the mixture was stirred at room temperature for one hour. The reaction solution was concentrated, water was added, extraction was performed with ether and the organic layer was further washed with aqueous sodium thiosulfate, water and saturated saline. After drying over magnesium sulfate and vacuum concentration, the residue was purified with a silica gel column (hexane) to obtain 2,4,6-trimethylphenyldisulfide as a light yellow crystalline compound (231 mg, 0.76 mmol, 67% yield). The NMR and mass spectral data for the obtained compound were as follows:
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06900307B1 |
| 出典データセット | uspto-grants-2005_05 |
| ORD ID | ord-66600d1abbe64ed2958ff894b380c2be |
| 出典メモ | uspto-grants-2005_05 |