Sodium Cyanide → (4-Fluoro-2,6-dimethyl-phenyl)-acetonitrile
반응식
[CH3:1][C:2]1[CH:9]=[C:8]([F:10])[CH:7]=[C:6]([CH3:11])[C:3]=1[CH2:4]Br.[C-:12]#[N:13].[Na+]>C(O)C.O>[F:10][C:8]1[CH:9]=[C:2]([CH3:1])[C:3]([CH2:4][C:12]#[N:13])=[C:6]([CH3:11])[CH:7]=1참가 물질
4
실험 절차
A solution of 1.86 g (9 mmol) 2,6-dimethyl-4-fluoro-benzyl bromide and 0.420 g (9 mmol) sodium cyanide in 21 ml ethanol/water 6:1 was heated to reflux for 4h. The cooled reaction mixture was concentrated and extracted with ethyl acetate. The combined extracts were washed with brine, dried over Na2SO4, filtered and evaporated. Filtration of the residue through a silica gel pad with heptane/ethyl acetate 1:1 provided (4-fluoro-2,6-dimethyl-phenyl)-acetonitrile as colourless solid: MS (EI): 163.1 (M+.), 148.1 ((M-CH3)+.), 136.1 ((M-HCN)+., 100%).
후처리
- temperatureto reflux for 4h
- customThe cooled reaction mixture
- concentrationwas concentrated
- extractionextracted with ethyl acetate
- washThe combined extracts were washed with brine
- dry with materialdried over Na2SO4
- filtrationfiltered
- customevaporated
- filtrationFiltration of the residue through a silica gel pad with heptane/ethyl acetate 1:1 provided (4-fluoro-2,6-dimethyl-phenyl)-acetonitrile as colourless solid
출처 및 근거
- ORD 기록
- ord-5d0223a8eac8424f8f1fabe3869f7d23
- 출처 데이터셋
- uspto-grants-2011_01
- 특허 번호
- US07875645B2
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