反应详情

2-Propoxy-4-(trifluoromethyl)benzoic acid (457 mg, 1.93 mmol) in THF was reacted with N,O-dimethylhydroxy amine (378 mg), NMM (0.65 ml) and DMTMM (947 mg) at room temperature overnight. The reaction solvent was removed in vacuo. Water (30 ml) was added to the resulting residue, which was extracted with ethyl acetate (30 ml×3). The combined organic layer was washed with 1 M NaHCO3 (30 ml), 1N HCl (30 ml) and brine (30 ml) and dried over MgSO4. The filterate was purified with column chromatography (Hex/EtOAc=4/1) to yield the title compound (277 mg, 49%).

1. customThe reaction solvent was removed in vacuo
2. additionWater (30 ml) was added to the resulting residue, which
3. extractionwas extracted with ethyl acetate (30 ml×3)
4. washThe combined organic layer was washed with 1 M NaHCO3 (30 ml), 1N HCl (30 ml) and brine (30 ml)
5. dry with materialdried over MgSO4
6. customThe filterate was purified with column chromatography (Hex/EtOAc=4/1)