Dimethylformamide → 4-Fluorobenzonitrile
反応式
[F:1][C:2]1[CH:3]=[CH:4][C:5](C(F)(F)F)=[C:6]([CH:9]=1)C#N.C([O-])([O-])=O.[K+].[K+].C[N:21]([CH:23]=O)C>O>[F:1][C:2]1[CH:3]=[CH:4][C:5]([C:23]#[N:21])=[CH:6][CH:9]=1参加物
5
実験手順
5-FLUORO-2-(TRIFLUOROMETHYL)BENZONITRILE (compound 8h; Oakwood), K2CO3 (4 eq.) and DMF (5 mL) was shaken at 110° C. for 16 h. After cooling to room temperature, the mixture was diluted with water (20 mL), extracted with CHCl3 (3×20 mL), and concentrated. The residue was dissolved in THF/MeOH (10 mL/4 mL), and treated with HCl (1N, 3 mL) at room temperature for 12 h. The solvent was evaporated and the residue was diluted with CHCl3 (20 mL), neutralized with NH4OH (28% aqueous) and purified by column chromatography (CH3Cl/MeOH 10/1) to give:
後処理
- extractionextracted with CHCl3 (3×20 mL)
- concentrationconcentrated
- dissolutionThe residue was dissolved in THF/MeOH (10 mL/4 mL)
- additiontreated with HCl (1N, 3 mL) at room temperature for 12 h
- customThe solvent was evaporated
- additionthe residue was diluted with CHCl3 (20 mL)
- custompurified by column chromatography (CH3Cl/MeOH 10/1)
- customto give
出典と根拠
- ORDレコード
- ord-2aa16be51f2b4889b4f1b9cb99afa292
- 出典データセット
- uspto-grants-2015_06
- 特許番号
- US09056832B2
反応ノート
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