Ammonium Chloride → HCID 69448738、化合物
反応式
[CH3:1][O:2][C:3](=[O:15])[C:4]1[CH:9]=[CH:8][C:7]([CH2:10][OH:11])=[C:6]([N+:12]([O-])=O)[CH:5]=1.[NH4+].[Cl-]>CCO.[Fe]>[CH3:1][O:2][C:3](=[O:15])[C:4]1[CH:9]=[CH:8][C:7]([CH2:10][OH:11])=[C:6]([NH2:12])[CH:5]=1参加物
5
反応条件
- 温度
- 75 °C
実験手順
To a solution of 4-hydroxymethyl-3-nitro-benzoic acid methyl ester (step (b), 5.6 g, 26.5 mmol) in 60 mL EtOH/30 mL H2O was added Fe powder (7.5 g, 134.3 mmol) and NH4Cl (0.75 g, 14.0 mmol). The reaction mixture was stirred at 75° C. for 3 h, then filtered while hot through Celite. The Celite was washed with EtOAc and MeOH. The filtrate was concentrated in vacuo and partitioned between EtOAc/H2O. The EtOAc layers was dried over MgSO4 and concentrated in vacuo to give a yellow solid. MS m/z: 179.9 (M−1).
後処理
- filtrationfiltered while hot through Celite
- washThe Celite was washed with EtOAc and MeOH
- concentrationThe filtrate was concentrated in vacuo
- custompartitioned between EtOAc/H2O
- dry with materialThe EtOAc layers was dried over MgSO4
- concentrationconcentrated in vacuo
- customto give a yellow solid
出典と根拠
- ORDレコード
- ord-9541bd7d11414f3d88b88300ebd087e1
- 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…