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Sodium Iodide → 3,4-Dimethoxyphenyldisulfide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Iodide | HCID 5238 | — |
| 反応物 | Acetic acid, 2-fluoro-, 1,1'-anhydride | HCID 67886 | — |
| 反応物 | 3,4-Dimethoxybenzenesulfonyl chloride | HCID 2734183 | — |
| 溶媒 | Acetone | HCID 180 | — |
| 生成物 | 3,4-Dimethoxyphenyldisulfide | HCID 11267746 | — |
反応手順
3,4-dimethoxyphenylsulfonyl chloride (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 3,4-dimethoxyphenyldisulfide as a light yellow crystalline compound (58% 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-03b07f8954b243fda6cc6cb8b2bc2cb9 |
| 出典メモ | uspto-grants-2005_05 |