Boron tribromide → 2,6-Difluoro-3-hydroxybenzonitrile
反応式
[F:1][C:2]1[C:9]([O:10]C)=[CH:8][CH:7]=[C:6]([F:12])[C:3]=1[C:4]#[N:5].B(Br)(Br)Br>C(Cl)Cl>[F:1][C:2]1[C:9]([OH:10])=[CH:8][CH:7]=[C:6]([F:12])[C:3]=1[C:4]#[N:5]参加物
4
実験手順
2,6-difluoro-3-methoxybenzonitrile (4.42 g, 26.1 mmol) was dissolved in DCM (10 mL) at 0° C. then 1 M BBr3 (52.2 mL, 52.2 mmol) was added. The reaction mixture was then warmed up to RT and stirred overnight. The reaction mixture was poured into ice water and extracted with more DCM. The organic layer was separated, dried over Na2SO4, filtered, and evaporated to dryness to yield 2,6-difluoro-3-hydroxybenzonitrile: LC-MS: M+1=156.
後処理
- extractionextracted with more DCM
- customThe organic layer was separated
- dry with materialdried over Na2SO4
- filtrationfiltered
- customevaporated to dryness
出典と根拠
- ORDレコード
- ord-8c287bd2ca46486b80208d0799ea52f3
- 出典データセット
- uspto-grants-2015_12
- 特許番号
- US09206199B2
反応ノート
読み込み中…