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Sodium Chloride → Pyridine-3-sulfonyl chloride
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Chloride | HCID 5234 | — |
| 反応物 | Phosphorus oxychloride | HCID 24813 | — |
| 反応物 | Phosphorus pentachloride | HCID 24819 | — |
| 反応物 | 3-Pyridinesulfonic acid | HCID 69468 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 溶媒 | tert-Butyl methyl ether | HCID 15413 | — |
| 生成物 | Pyridine-3-sulfonyl chloride | HCID 3164136 | 94.3% |
反応手順
A mixture of pyridine-3-sulfonic acid (10.3 g, 64.8 mmol), phosphorus pentachloride (20.82 g, 100 mmol) and phosphorus oxychloride (10 mL, 109 mmol) was heated to reflux for 3 h (according to J. Org. Chem. 1989, 54(2), 389.). Evaporated to dryness to give a yellow solid, dissolved in ice water and methyl-tert-butyl ether, added cautiously sat. NaHCO3-sol. until neutralized, saturated with solid NaCl, separated phases, dried organic layer over Na2SO4. Removal of the solvent in vacuum to give the title compound as an orange liquid (10.85 g, 94%). MS (ISP) 178.1 [(M+H)+] and 180.0 [(M+2+H)+].
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07446113B2 |
| 出典データセット | uspto-grants-2008_11 |
| ORD ID | ord-f04bdb6b900a43cb9eb113fee6b6c913 |
| 出典メモ | uspto-grants-2008_11 |