Thionyl Chloride → 2-Chloro-4-fluoro-1,3-benzoxazole
反応式
[F:1][C:2]1[C:7]2[N:8]=[C:9](S)[O:10][C:6]=2[CH:5]=[CH:4][CH:3]=1.S(Cl)([Cl:14])=O>CN(C)C=O>[Cl:14][C:9]1[O:10][C:6]2[CH:5]=[CH:4][CH:3]=[C:2]([F:1])[C:7]=2[N:8]=1参加物
4
実験手順
To a solution of 560 mg (3.31 mmol) 4-fluoro-benzooxazole-2-thiol in 3.6 mL (49.65 mmol) thionyl chloride was added dropwise 60.3 □L N,N-dimethylformamide dry at room temperature. The mixture was stirred at room temperature for 2.5 h. The solvent was removed in vacuo. The crude compound was purified with flash column chromatography on silica eluting with a gradient formed from n-heptane and ethyl acetate to provide 434 mg (76.4%) of the title compound as a white solid. MS(m/e): 171 (M+H+).
後処理
- customdry at room temperature
- customThe solvent was removed in vacuo
- customThe crude compound was purified with flash column chromatography on silica eluting with a gradient
- customformed from n-heptane and ethyl acetate
出典と根拠
- ORDレコード
- ord-19c1ce3755954d03952a270a6c3038b7
- 出典データセット
- uspto-grants-2011_03
- 特許番号
- US07897627B2
反応ノート
読み込み中…