反应详情

To a stirred solution of 1,2-bis(methyloxy)-4-{[(methyloxy)methyl]oxy}benzene (4.0 g) and TMEDA (3.93 ml) in dry diethyl ether (50 ml) was added tert-butyllithium (1.7M in pentane, 23.76 ml) at −70 C. The reaction was stirred at this temperature for 1 h before adding bromine (0.15 ml). This was allowed to stir at 0 C for 3 h. The reaction was quenched by addition of 20% aqueous sodium dithionite and extracted with ethyl acetate. The organics were washed with dilute hydrochloric acid, aqueous sodium bicarbonate, brine and dried over sodium sulphate to yield a crude product. This was purified through silica, eluting with 0-10% ethyl acetate in hexane to give the title compound, 1.4 g

1. stirringto stir at 0 C for 3 h
2. customThe reaction was quenched by addition of 20% aqueous sodium dithionite
3. extractionextracted with ethyl acetate
4. washThe organics were washed with dilute hydrochloric acid, aqueous sodium bicarbonate, brine
5. dry with materialdried over sodium sulphate
6. customto yield a crude product
7. customThis was purified through silica
8. washeluting with 0-10% ethyl acetate in hexane