Water → 4-(Bromomethyl)-3,5-difluoropyridine
반응식
[F:1][C:2]1[CH:3]=[N:4][CH:5]=[C:6]([F:10])[C:7]=1[CH2:8]O.P(Br)(Br)[Br:12].O>C(Cl)(Cl)Cl>[Br:12][CH2:8][C:7]1[C:2]([F:1])=[CH:3][N:4]=[CH:5][C:6]=1[F:10]참가 물질
5
실험 절차
To a solution of (3,5-difluoropyridin-4-yl)methanol (3.5 mmol) in anhydrous chloroform (15 mL) was added dropwise a solution of phosphorus tribromide (330 μL, 3.5 mmol) in anhydrous chloroform (5 mL) at 0° C. The mixture was stirred for 6 hours at room temperature. Water was added, and the reaction was extracted 3 times with dichloromethane. The combined organic phases were washed with brine and dried over magnesium sulfate. After evaporation of the solvent, 4-(bromomethyl)-3,5-difluoropyridine was obtained as pale yellow solid (600 mg, 83% yield for 2 steps) and used in the next step without purification; 1H NMR (400 MHz, MeOd4): δ 4.59 (s, 2H), 8.42 (s, 2H).
후처리
- extractionthe reaction was extracted 3 times with dichloromethane
- washThe combined organic phases were washed with brine
- dry with materialdried over magnesium sulfate
- customAfter evaporation of the solvent
출처 및 근거
- ORD 기록
- ord-802b32d49c4a4d679b677987b93b47a5
- 출처 데이터셋
- uspto-grants-2015_05
- 특허 번호
- US09040538B2
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