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18-Crown-6 → 3-Chloro-4-fluorobenzenesulfonyl fluoride
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 18-Crown-6 | HCID 28557 | — |
| 反応物 | 3-Chloro-4-fluorobenzenesulphonyl chloride | HCID 145222 | — |
| 反応物 | Potassium Fluoride | HCID 522689 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 3-Chloro-4-fluorobenzenesulfonyl fluoride | HCID 20511714 | — |
反応手順
To a solution of the commercially available 3-chloro-4-fluorobenzenesulfonyl chloride (7 g, 30 mmol) in CH3CN (40 mL) was added KF (7 g, 120 mmol) and 18-crown-6 (0.5 g), then the mixture was stirred at room temperature overnight. The mixture was quenched with aqueous water and extracted with EtOAc, the organic layer was washed with brine, dried over anhydrous Na2SO4, concentrated to give the crude product which was purified by column to give the reagent R-12a (4.2 g, 95.5%) as a pale yellow solid. ESI-MS (M+1): 213.2 calc. for C6H3CIF2O2S
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09440989B2 |
| 出典データセット | uspto-grants-2016_09 |
| ORD ID | ord-4d2f9af19e2e475e8307933b0643585b |
| 出典メモ | uspto-grants-2016_09 |