Hydrogen Bromide → HCID 14450998、化合物
反応式
C[O:2][C:3]1[C:10]([O:11]C)=[CH:9][C:8]([N+:13]([O-:15])=[O:14])=[CH:7][C:4]=1[CH:5]=[O:6].Br>C(O)(=O)C>[OH:2][C:3]1[C:10]([OH:11])=[CH:9][C:8]([N+:13]([O-:15])=[O:14])=[CH:7][C:4]=1[CH:5]=[O:6]参加物
4
実験手順
10.0 g of 2,3-dimethoxy-5-nitrobenzaldehyde are treated with 50 ml of glacial acetic acid and 50 ml of constant-boiling hydrobromic acid and held at the reflux temperature for 7 hours. After treatment with ice the separated precipitate is filtered under suction, washed with water and taken up in ethyl acetate. The organic phase is dried over sodium sulfate and evaporated. The crude product obtained is filtered over silica gel with ethyl acetate. After crystallization from ethyl acetate/hexane there is obtained 2,3-dihydroxy-5-nitrobenzaldehyde in the form of brownish crystals of m.p. 226°-228°.
後処理
- filtrationAfter treatment with ice the separated precipitate is filtered under suction
- washwashed with water
- dry with materialThe organic phase is dried over sodium sulfate
- customevaporated
- customThe crude product obtained
- filtrationis filtered over silica gel with ethyl acetate
- customAfter crystallization from ethyl acetate/hexane there
出典と根拠
- ORDレコード
- ord-92f28bfd8ce349898c350e2c071e0ffe
- 出典データセット
- uspto-grants-1997_05
- 特許番号
- US05633371
反応ノート
読み込み中…