反应详情

A mixture of 4-fluoro phenyl acetic acid (2 g, 13 mmol), 3,4,5 trimethoxybenzaldehyde (2.5 g, 13 mmol), Ac2O (10 mL) and DIPEA (2.9 mL, 16.8 mmol) was stirred at room temperature for 12 hours. Upon completion, as monitored by TLC using DCM:MeOH (9:1) as the eluent, 10% aqueous HCl (10 mL) was added to the reaction mixture; the precipitate formed was filtered and dissolved in DCM (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 100 mL water and dried to get the product (2.4 g, 56% yield).

1. additionwas added to the reaction mixture
2. customthe precipitate formed
3. filtrationwas filtered
4. dissolutiondissolved in DCM (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 100 mL water
9. customdried