反应详情

Stir a solution of 5-(2,2-difluorovinyl)-N-methyl-N-propyl-isophthalamic acid ethyl ester (187 mg, 0.63 mmol), 1 N lithium hydroxide (2.5 mL, 2.5 mmol) and THF (2.5 mL) at room temperature overnight. Partition the reaction between ethyl acetate and water. Acidify the aqueous with 5 N HCl and extract with ethyl acetate. Dry (magnesium sulfate), concentrate and purify (silica gel chromatography, eluting with 2:98 to 6:94 methanol:dichloromethane with 1% acetic acid) to give the title compound (78 mg, 44%).

1. customPartition
2. customthe reaction between ethyl acetate and water
3. extractionextract with ethyl acetate
4. dry with materialDry (magnesium sulfate)
5. concentrationconcentrate
6. custompurify
7. wash(silica gel chromatography, eluting with 2:98 to 6:94 methanol:dichloromethane with 1% acetic acid)