反应详情

A mixture of 2-methoxy-5-nitro-benzoic acid (2.00 g, 10.1 mmol), HATU (3.86 g, 10.1 mmol), TEA (4.23 mL) and 100 mL THF was stirred for 30 min. Then 4-bromoaniline (1.75 g, 10.1 mmol) was added and the mixture was stirred for 3 days and concentrated. The crude material was dissolved in EtOAc and the organic phase was washed with satd. aq. NaHCO3. The precipitate was collected and again dissolved in EtOAc and washed with water and satd. NaHCO3. The organic phase was dried with Na2SO4, filtered and concentrated to furnish the subtitle compound. Yield: 930 mg (26%). MS [M+H]+=351 (Br-isotope pattern); TLC: Rf=0.94 (silica gel, DCM:EtOH 9:1).

1. stirringthe mixture was stirred for 3 days
2. concentrationconcentrated
3. dissolutionThe crude material was dissolved in EtOAc
4. washthe organic phase was washed with satd
5. customThe precipitate was collected
6. dissolutionagain dissolved in EtOAc
7. washwashed with water
8. dry with materialThe organic phase was dried with Na2SO4
9. filtrationfiltered
10. concentrationconcentrated