Methanol → Methyl 4-(hydroxymethyl)-3-nitrobenzoate
反応式
[OH:1][CH2:2][C:3]1[CH:11]=[CH:10][C:6]([C:7]([OH:9])=[O:8])=[CH:5][C:4]=1[N+:12]([O-:14])=[O:13].[CH3:15]O>OS(O)(=O)=O>[CH3:15][O:8][C:7](=[O:9])[C:6]1[CH:10]=[CH:11][C:3]([CH2:2][OH:1])=[C:4]([N+:12]([O-:14])=[O:13])[CH:5]=1参加物
4
反応条件
- 温度
- 70 °C
実験手順
4-Hydroxymethyl-3-nitro-benzoic acid (step (a), 2.0 g, 10.2 mmol) was dissolved in 100 mL of MeOH, treated with 10 drops of concentrated H2SO4 and stirred at 70° C. After 36 h, the solution was concentrated in vacuo and redissolved in EtOAc. The EtOAc solution was washed with 1N NaOH and brine, dried over MgSO4, and concentrated to afford the title compound as a light-yellow solid upon drying under vacuum. MS m/z: 210.1 (M−1).
後処理
- concentrationthe solution was concentrated in vacuo
- dissolutionredissolved in EtOAc
- washThe EtOAc solution was washed with 1N NaOH and brine
- dry with materialdried over MgSO4
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-91887a49dcbf4a5ebbb0ffbfe966507f
- 出典データセット
- uspto-grants-2004_11
- 特許番号
- US06822097B1
反応ノート
読み込み中…