Potassium Cyanide → 2-(3-Bromo-5-fluorophenyl)acetonitrile
반응식
[Br:1][C:2]1[CH:3]=[C:4]([CH:7]=[C:8]([F:10])[CH:9]=1)[CH2:5]Br.[C-:11]#[N:12].[K+]>O1CCOCC1.O.CCO>[Br:1][C:2]1[CH:3]=[C:4]([CH2:5][C:11]#[N:12])[CH:7]=[C:8]([F:10])[CH:9]=1참가 물질
6
실험 절차
To a solution of 3-bromo-5-fluorobenzyl bromide (3.2 g, 0.0112 mole) in 1,4-dioxane (20 mL) was added a solution of KCN (0.82 g, 0.013 mole) in H2O (5 mL) and EtOH (5 mL), refluxed for 2 hours. Extracted with ether, washed with brine, dried over MgSO4, concentrated. Column chromatography using hexane/ethyl acetate (19:1). 3-Bromo-5-fluorophenylacetonitrile obtained was a colorless oil: 1H NMR (DMSO-d6) d 4.15 ( s, 2H), 7.29( d, 1H, J=9.37 Hz), 7.47(s, 1H), 7.55(d, 1H, J=8.45 Hz); MS( EI) M+m/z 213; Anal. Calc. For C8H5BrFN: C, 44.89, H, 2.35, N,6.54. Found: C, 44.88, H, 2.32, N, 6.46.
후처리
- temperaturerefluxed for 2 hours
- extractionExtracted with ether
- washwashed with brine
- dry with materialdried over MgSO4
- concentrationconcentrated
출처 및 근거
- ORD 기록
- ord-9188853e41364cb3b508046fee101a2f
- 출처 데이터셋
- uspto-grants-2003_05
- 특허 번호
- US06566358B2
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