反应详情

温度

5 °C

A stirred mixture of 2,3-dichloroanisole (89 g., 0.50 mole) and 6-bromohexanoyl chloride (120 g., 0.59 mole) is methylene chloride (500 ml.) is cooled to 5° C. and treated with aluminum chloride (74 g., 0.56 mole) in portions during a one-half hour period. The reaction mixture is kept at 25° C. for 18 hours, then poured into ice water (1 liter) containing hydrochloric acid (100 ml.). The organic phase is separated, washed with water, 2% sodium hydroxide, and dilute hydrochloric acid. The methylene chloride is evaporated at reduced pressure, the residual oil dissolved in ether, dried over magnesium sulfate, evaporated to 200 ml. and treated with hexane (600 ml.) affording 2,3-dichloro-4-(6-bromohexanoyl)-anisole which melts at 52°-53° C.

1. customThe organic phase is separated
2. washwashed with water, 2% sodium hydroxide, and dilute hydrochloric acid
3. customThe methylene chloride is evaporated at reduced pressure
4. dissolutionthe residual oil dissolved in ether
5. dry with materialdried over magnesium sulfate
6. customevaporated to 200 ml
7. additionand treated with hexane (600 ml.)