反应详情

Chill a solution of 5-(difluorophenyl-methyl)-N-methyl-N-propyl-isophthalamic acid methyl ester (0.043 g, 0.119 mmol) in THF (1 mL) in an ice bath. Add 1 N lithium hydroxide (0.18 mL, 0.18 mmol) and stir at room temperature for 3 h. Acidify the solution to about pH=2 and concentrate to one half of the solvent. Partition the residue between ethyl acetate and H2O. Extract the aqueous layer with ethyl acetate (2×10 mL). Wash the combined organic extract with saturated aqueous sodium chloride, dry (magnesium sulfate) and concentrate to give the title compound (95%).

1. concentrationconcentrate to one half of the solvent
2. customPartition the residue between ethyl acetate and H2O
3. extractionExtract the aqueous layer with ethyl acetate (2×10 mL)
4. washWash the combined
5. extractionorganic extract with saturated aqueous sodium chloride
6. dry with materialdry (magnesium sulfate)
7. concentrationconcentrate