反应详情

To a well stirred solution of Methyl-2-bromomethyl-7-methoxybenzo[b]furan-4-carboxylate (step 6) (3.1 g, 10.36 mmol) in dimethyl sulfoxide (30.0 mL) was added powdered sodium carbonate (1.64 g, 15.55 mmol) at 90-95° C. and stirred for 2-3 hours. Reaction mixture was cooled to room temperature and diluted with water (300 mL) and extracted with ethyl acetate (3×100 mL). The combined organic layers were washed with water (2×50 mL) and dried over anhydrous sodium sulfate. Removal of solvent gave crude product (2.9 g) as brown viscous oil. Purification by silica gel column using chloroform: ethyl acetate (95:5) as an eluent afforded 2.2 g of pure product.

1. customReaction mixture
2. extractionextracted with ethyl acetate (3×100 mL)
3. washThe combined organic layers were washed with water (2×50 mL)
4. dry with materialdried over anhydrous sodium sulfate
5. customRemoval of solvent
6. customgave crude product (2.9 g) as brown viscous oil
7. customPurification by silica gel column