反应详情

9.7 ml of TiCl4 (2.1 eq) and 4.2 ml of dichloromethyl methyl ether (1.1 eq) are dissolved in 20 ml of dichloromethane at 0° C. A solution of 10 g of 2-bromo-6-methoxynapthalene (1 eq) is added dropwise in such a way that the temperature does not exceed 5° C. The reaction mixture is stirred at RT over night, followed by the addition of 300 ml of 1% HCl. The organic and aqueous phases are separated, and the aqueous phase is extracted with dichloromethane. The combined organic phases are washed with saturated sodium chloride solution, dried over magnesium sulfate and evaporated to dryness on a rotary evaporator to obtain the desired product in quantitative yield (11 g).

1. customdoes not exceed 5° C
2. customThe organic and aqueous phases are separated
3. extractionthe aqueous phase is extracted with dichloromethane
4. washThe combined organic phases are washed with saturated sodium chloride solution
5. dry with materialdried over magnesium sulfate
6. customevaporated to dryness on a rotary evaporator