Phosphorus tribromide → 4-(Bromomethyl)-3,5-difluorobenzonitrile
反応式
[F:1][C:2]1[CH:3]=[C:4]([CH:7]=[C:8]([F:12])[C:9]=1[CH2:10]O)[C:5]#[N:6].P(Br)(Br)[Br:14]>C(Cl)Cl>[Br:14][CH2:10][C:9]1[C:2]([F:1])=[CH:3][C:4]([C:5]#[N:6])=[CH:7][C:8]=1[F:12]参加物
4
反応条件
- 温度
- 0 °C
実験手順
To a solution of 3,5-difluoro-4-(hydroxymethyl)benzonitrile (all material from above reaction) in DCM at 0° C. was added PBr3 (283 μL, 3 mmol). After stirring 1 h at 0° C., the reaction mixture was quenched with water and then extracted with DCM. The combined extracts were washed with satd NaHCO3, dried over Na2SO4 and concentrated to yield 4-(bromomethyl)-3,5-difluorobenzonitrile (0.88 g, 63%, combined yield) as a white solid. 1H NMR (400 MHz, CDCl3) δ 7.31-7.18 (m, 1H), 4.51 (d, J=10.1, 1H); GC-MS (ES) m/z 231 (M).
後処理
- customthe reaction mixture was quenched with water
- extractionextracted with DCM
- washThe combined extracts were washed with satd NaHCO3
- dry with materialdried over Na2SO4
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-014f40635230441b9d3cc0720c733e2e
- 出典データセット
- uspto-grants-2014_07
- 特許番号
- US08785488B2
反応ノート
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