関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 1-Fluoro-3-nitrobenzene | HCID 9823 | — |
| 反応物 | Chlorosuccinimide | HCID 31398 | — |
| 反応物 | Sodium bis(trimethylsilyl)amide | HCID 2724254 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 2-Chloro-1-fluoro-3-nitrobenzene | HCID 88883 | 9.3% |
反応手順
To a −78° C. solution of 3-fluoronitrobenzene (2 g, 14.2 mmol) in THF (30 mL) was added N-chlorosuccinimide (5.69 g, 42.6 mmol) in THF (20 mL), NaHMDS (1 M in THF, 28.4 mL, 28.4 mmol) was then added dropwise to maintain an internal temperature below −75° C. The resulting mixture was stirred for 30 min at −78° C. Then it was partitioned between 5% of HCl and ethyl acetate. The combined organic layer is dried over MgSO4 and filtered. The solvent was evaporated and chromatography of the resulting solid on silica gel (20% Ethyl acetate Hexane) gave the desired product(231 mg, 9.2%). EI-MS m/z 176.5 (M+).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06500863B1 |
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| 出典データセット | uspto-grants-2002_12 |
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| ORD ID | ord-024e256dfd614b48956879219a3257c2 |
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| 出典メモ | uspto-grants-2002_12 |
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