反应详情

2-Nitro-4-trifluoromethyl-benzoic acid (2.753 mg, 11.7 mmol) in THF was reacted with N,O-dimethylhydroxy amine (1.277 g, 13.1 mmol), NMM (3 ml) and DMTMM (3.34 g) at room temperature overnight. The reaction mixture was quenched by adding H2O. The mixture was extracted with ethyl acetate (50 ml×3). The combined organic layer was washed 1M NaHCO3 (50 ml×2), 3% HCl (50 ml×2) and brine (50 ml), and then dried over MgSO4. The filterate was concentrated in vacuo to yield the title compound (2.84 g, 87%).

1. customThe reaction mixture was quenched
2. additionby adding H2O
3. extractionThe mixture was extracted with ethyl acetate (50 ml×3)
4. washThe combined organic layer was washed 1M NaHCO3 (50 ml×2), 3% HCl (50 ml×2) and brine (50 ml)
5. dry with materialdried over MgSO4
6. concentrationThe filterate was concentrated in vacuo