反応式
[CH:1]([C:3]1[C:4]([CH3:12])=[C:5]([C:8]([F:11])=[CH:9][CH:10]=1)[C:6]#[N:7])=[CH2:2].C1C=C(Cl)C=C(C(OO)=[O:21])C=1>C(Cl)Cl>[F:11][C:8]1[C:5]([C:6]#[N:7])=[C:4]([CH3:12])[C:3]([CH:1]2[CH2:2][O:21]2)=[CH:10][CH:9]=1参加物
4
実験手順
3-Ethenyl-6-fluoro-2-methylbenzonitrile (14.9 g, 92.0 mmol) was added to DCM (400 mL) at 0° C. then mCPBA (47.85 g, 277.5 mmol) was added and the mixture was stirred at RT for 72 h. The reaction mixture was washed with saturated aqueous Na2S2O3, then with 1N NaOH, and brine. The organic layer was separated, dried over Na2SO4, filtered, and evaporated to dryness. The crude product was purified by chromatography through a 330 g Redi-sep column, eluting with 0-100% hexane/DCM solvent system to afford 6-fluoro-2-methyl-3-(oxiran-2-yl)benzonitrile. LC-MS: M+1=178.
後処理
- washThe reaction mixture was washed with saturated aqueous Na2S2O3
- customThe organic layer was separated
- dry with materialdried over Na2SO4
- filtrationfiltered
- customevaporated to dryness
- customThe crude product was purified by chromatography through a 330 g Redi-sep column
- washeluting with 0-100% hexane/DCM solvent system
出典と根拠
- ORDレコード
- ord-ece37e959a7b494f8a59842fed09652b
- 出典データセット
- uspto-grants-2015_12
- 特許番号
- US09206199B2
関連ノート
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