Methyl 5-methoxy-2-nitrobenzoate → 5-Methoxy-2-nitrobenzoic acid
反応式
C[O:2][C:3](=[O:15])[C:4]1[CH:9]=[C:8]([O:10][CH3:11])[CH:7]=[CH:6][C:5]=1[N+:12]([O-:14])=[O:13]>C(O)C.[OH-].[Na+]>[CH3:11][O:10][C:8]1[CH:7]=[CH:6][C:5]([N+:12]([O-:14])=[O:13])=[C:4]([CH:9]=1)[C:3]([OH:15])=[O:2]参加物
4
実験手順
The crude material from Example 44b (23.3 g) is dissolved in 110 ml ethanol and 44 ml of 4N NaOH. The mixture is stirred at rt for 18 h. After that time, the ethanol is evaporated. To the residue, water is added and the mixture is washed twice with dichloromethane. To the water phase, conc. HCl is added until pH=1 is reached. The title compound is obtained by extraction with ether. Purification follows by crystallization from ethyl acetate-hexane. mp: 131-134° C.; MS: 196 (M+−1); HPLC: tret=7.90 min (Grad 1).
後処理
- customAfter that time, the ethanol is evaporated
- additionTo the residue, water is added
- washthe mixture is washed twice with dichloromethane
- additionTo the water phase, conc. HCl is added until pH=1
出典と根拠
- ORDレコード
- ord-d4fc026c49264179b6c8cb3a7f6c1101
- 出典データセット
- uspto-grants-2011_08
- 特許番号
- US07998972B2
反応ノート
読み込み中…