化工社化工社 化学情報印刷レポート · 研究参考用
Iodine → N-(5-iodo-2,3-dihydro-1H-inden-2-yl)-2-propanesulfonamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Iodine | HCID 807 | — |
| 反応物 | Sulfuric Acid | HCID 1118 | — |
| 反応物 | Metaperiodic acid | HCID 65185 | — |
| 反応物 | N-(2,3-dihydro-1H-inden-2-yl)-2-propanesulfonamide | HCID 46899808 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | N-(5-iodo-2,3-dihydro-1H-inden-2-yl)-2-propanesulfonamide | HCID 46899809 | 483.7% |
反応手順
Intermediate 1 (1.75 g, 7.32 mmol) was dissolved in glacial acetic acid (30 ml) and then treated with concentrated sulfuric acid (0.8 ml) followed by water (2.8 ml) with stirring. This mixture was then treated with periodic acid (0.23 eq., 0.38 g, 1.67 mmol) then iodine (0.43 eq., 800 mg, 3.15 mmol), and the whole mix was stirred at 60° C. for 3-4 h. The reaction mixture was allowed to cool and then partitioned between ethyl acetate and 10% aqueous sodium metabisulfite. The organic layer was separated and dried over sodium sulphate and evaporated in vacuo to give the title compound as a yellow oil (2.95 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07618969B2 |
| 出典データセット | uspto-grants-2009_11 |
| ORD ID | ord-ac14732020c64a43b96a3461b9d59c79 |
| 出典メモ | uspto-grants-2009_11 |