反应详情

温度

75 °C

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).

1. filtrationfiltered while hot through Celite
2. washThe Celite was washed with EtOAc and MeOH
3. concentrationThe filtrate was concentrated in vacuo
4. custompartitioned between EtOAc/H2O
5. dry with materialThe EtOAc layers was dried over MgSO4
6. concentrationconcentrated in vacuo
7. customto give a yellow solid