Nitric Acid → (4-Hydroxy-3-nitro-phenoxy)-acetonitrile
反応式
[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]参加物
5
実験手順
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.
後処理
- 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)
出典と根拠
- ORDレコード
- ord-17a2368ef58c408d9b99370d47afeb2f
- 出典データセット
- uspto-grants-1999_09
- 特許番号
- US05952362
反応ノート
読み込み中…