反応式
[F:1][C:2]1[CH:3]=[C:4]([N+:8]([O-:10])=[O:9])[CH:5]=[CH:6][CH:7]=1.[Cl:11]N1C(=O)CCC1=O.C[Si]([N-][Si](C)(C)C)(C)C.[Na+]>C1COCC1>[Cl:11][C:3]1[C:2]([F:1])=[CH:7][CH:6]=[CH:5][C:4]=1[N+:8]([O-:10])=[O:9]参加物
5
反応条件
- 温度
- -78 °C
実験手順
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+).
後処理
- additionwas then added dropwise
- temperatureto maintain an internal temperature below −75° C
- customThen it was partitioned between 5% of HCl and ethyl acetate
- dry with materialThe combined organic layer is dried over MgSO4
- filtrationfiltered
- customThe solvent was evaporated
出典と根拠
- ORDレコード
- ord-024e256dfd614b48956879219a3257c2
- 出典データセット
- uspto-grants-2002_12
- 特許番号
- US06500863B1
関連ノート
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