反应详情

6-Bromo-2-naphthol (25.33 g) was suspended in dichloromethane (300 ml) and titanium tetrachloride (25.0 ml) was slowly added dropwise under cooling in an ice bath. 1,1-Dichloromethylmethyl ether (10.5 ml) was added dropwise to the reaction mixture and the mixture was stirred at the same temperature for 1 hr. The reaction mixture was poured into iced water and dichloromethane was added. The organic layer was separated and the aqueous layer was extracted with dichloromethane. The combined organic layers were washed successively with IN hydrochloric acid, water and saturated aqueous sodium hydrogen carbonate, dried over anhydrous magnesium sulfate and concentrated to give the title compound (28.17 g) as brown crystals.

1. temperatureunder cooling in an ice bath
2. additionwas added
3. customThe organic layer was separated
4. extractionthe aqueous layer was extracted with dichloromethane
5. washThe combined organic layers were washed successively with IN hydrochloric acid, water and saturated aqueous sodium hydrogen carbonate
6. dry with materialdried over anhydrous magnesium sulfate
7. concentrationconcentrated