反应详情

To a well stirred solution of Methyl-2-formyl-7-methoxybenzo[b]furan-4-carboxylate (from step 7) (2.0 g, 8.53 mmol) in toluene (50.0 mL) was added malonic acid (1.33 g, 12.80 mmol) and Piperidine (0.5 ml). The reaction mixture was then refluxed for 3-4 hours. Reaction mixture was cooled to room temperature, acidified with 10% aqueous HCl solution and extracted with ethyl acetate (2×100 mL). The combined organic layers were washed with water (2×100 mL0 and dried over anhydrous sodium sulfate. Removal of solvent under vacuo gave product (1.8 g) as light yellow solid.

1. temperatureThe reaction mixture was then refluxed for 3-4 hours
2. customReaction mixture
3. extractionextracted with ethyl acetate (2×100 mL)
4. washThe combined organic layers were washed with water (2×100 mL0
5. dry with materialdried over anhydrous sodium sulfate
6. customRemoval of solvent under vacuo