反应详情

A mixture of 4-fluorophenylacetic acid (2 g, 13 mmol), 3,4-difluorobenzaldehyde (2.5 g, 13 mmol), Ac2O (10 mL) and diisopropylethylamine (2.9 mL) was stirred at room temperature for 12 hours. Upon completion, as monitored by TLC using DCM:MeOH (9:1) as the eluent, 10 mL 10% aqueous HCl was added to the reaction mixture, the precipitate formed was filtered and dissolved in CH2Cl2 (100 mL). The organic layer was washed with 10% aqueous NaOH (3×50 mL) and the basic aqueous solution was acidified with 10% aqueous HCl to pH 3. The precipitate formed was filtered, washed with water (100 mL) and dried to get the product (4.4 g, 41.5% yield).

1. additionwas added to the reaction mixture
2. customthe precipitate formed
3. filtrationwas filtered
4. dissolutiondissolved in CH2Cl2 (100 mL)
5. washThe organic layer was washed with 10% aqueous NaOH (3×50 mL)
6. customThe precipitate formed
7. filtrationwas filtered
8. washwashed with water (100 mL)
9. customdried