反应详情

A solution of 1,2-dimethoxy-4,5-dinitrobenzene (500 mg, 2.19 mmol) in MeOH (10 mL) was degassed and put under N2 atmosphere. A catalytic amount of Pd on charcoal (10%) was quenched with MeOH (1 mL) and transferred in one shot as a suspension in MeOH into the solution. Acetic acid (1.5 mL) was added and the black mixture was put under H2 atmosphere (1 atm), stirred at rt for 16 h. The mixture was filtered through a celite pad and rinsed with MeOH. The filtrate was concentrated in vacuo at 80° C. to afford the title compound 182 (residual acetic acid could not be removed from the product). 1H NMR: (DMSO-d6) δ(ppm): 6.23 (s, 2H), 3.56 (s, 6H). m/z: 169.3. (MH+).

1. customA catalytic amount of Pd on charcoal (10%) was quenched with MeOH (1 mL)
2. additionAcetic acid (1.5 mL) was added
3. filtrationThe mixture was filtered through a celite pad
4. washrinsed with MeOH
5. concentrationThe filtrate was concentrated in vacuo at 80° C.