Nitric Acid → (4-Hydroxy-3-nitro-phenoxy)-acetonitrile
반응식
[OH:1][C:2]1[CH:11]=[CH:10][C:5]([O:6][CH2:7][C:8]#[N:9])=[CH:4][CH:3]=1.[N+:12]([O-])([OH:14])=[O:13].C(OCC)(=O)C>[N+](C)([O-])=O>[OH:1][C:2]1[CH:3]=[CH:4][C:5]([O:6][CH2:7][C:8]#[N:9])=[CH:10][C:11]=1[N+:12]([O-:14])=[O:13]참가 물질
5
실험 절차
A solution of 7.5 g of (4-hydroxy-phenoxy)-acetonitrile dissolved in 60 ml of nitromethane was cooled in an ice bath and 3.88 ml of 70% nitric acid was added dropwise. After 45 minutes, the reaction mixture was poured into ethyl acetate, washed with brine, dried (MgSO4), and evaporated to dryness. The crude product was purified by silica gel chromatography eluting with ethyl acetate/hexane (1:3), giving 5.45 g of (4-hydroxy-3-nitro-phenoxy)-acetonitrile as a yellow solid, mp 113.1-114.1° C.
후처리
- temperaturewas cooled in an ice bath
- washwashed with brine
- dry with materialdried (MgSO4)
- customevaporated to dryness
- customThe crude product was purified by silica gel chromatography
- washeluting with ethyl acetate/hexane (1:3)
출처 및 근거
- ORD 기록
- ord-17a2368ef58c408d9b99370d47afeb2f
- 출처 데이터셋
- uspto-grants-1999_09
- 특허 번호
- US05952362
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