反应详情

To a well stirred solution of 7-methoxy-2-methylbenzo[b]furan (72 g, 0.443 moles) in DCM (1.5 L) was added stannous chloride (150.3 g, 0.577 moles) followed by slow addition of 1,1-dichloromethyl methyl ether (56.1 g, 0.488 moles) at −10-0° C. and stirred for 1-2 hrs. Ice cold water (1.0 L) was added with vigorous stirring, the organic layer was separated and washed with water (2×550 mL) and dried over anhydrous sodium sulfate. Removal of solvent gave crude product (68.0 g). The crude product was purified by silica gel column using petroleum ether: ethyl acetate (9:1) as an eluent to afford the product as pale yellow oil (52 g).

1. customthe organic layer was separated
2. washwashed with water (2×550 mL)
3. dry with materialdried over anhydrous sodium sulfate
4. customRemoval of solvent
5. customgave crude product (68.0 g)
6. customThe crude product was purified by silica gel column