反应详情

The mixture of (2,4,5-trichloro-phenoxyacetic acid (127.8 mg, 0.5 mmol), 3-aminobenzoic acid methyl ester (151.2 mg, 1.0 mmol), 4-dimethylaminopyridine (122.2 mg, 1.0 mmol) and benzotriazole-1-yl-oxy-tris-pyrrolidino-phosphonium hexafluorophosphate (pybop) (520.3 g, 1.0 mmol) in DMF (5.0 mL) was stirred overnight and then partitioned between ethyl acetate and 10% HCl. The organic phase was washed with brine, dried (MgSO4 anh), and concentrated. The residue was purified by silica gel flash column chromatography (n-Hexane:Ethyl acetate:MeOH=6:3:1) to give 3-[2-(2,4,5-trichloro-phenoxy)-acetylamino]-benzoic acid methyl ester as a white solid (166.4 mg, 85.6% yield).

1. custompartitioned between ethyl acetate and 10% HCl
2. washThe organic phase was washed with brine
3. dry with materialdried (MgSO4 anh)
4. concentrationconcentrated
5. customThe residue was purified by silica gel flash column chromatography (n-Hexane:Ethyl acetate:MeOH=6:3:1)