Phosphorus tribromide → 4-(Bromomethyl)-3,5-difluorobenzonitrile
반응식
[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]참가 물질
4
반응 조건
- 온도
- 0 °C
실험 절차
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).
후처리
- customthe reaction mixture was quenched with water
- extractionextracted with DCM
- washThe combined extracts were washed with satd NaHCO3
- dry with materialdried over Na2SO4
- concentrationconcentrated
출처 및 근거
- ORD 기록
- ord-014f40635230441b9d3cc0720c733e2e
- 출처 데이터셋
- uspto-grants-2014_07
- 특허 번호
- US08785488B2
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