反应详情

A solution of sodium hydroxide (0.52 g.) in ethanol (50 ml.) was added dropwise to a stirred solution of 6-hydroxy-2,4-bis(trichloromethyl)benzo[1,3]dioxin (5 g.) in ethanol (100 ml.) and the resulting solution was stirred for 15 minutes. Methyl iodide (1.7 ml.) was then added, the reaction mixture was warmed on a steam bath for 1 hour, and evaporated to dryness under reduced pressure, and the oily residue was triturated with diethyl ether and filtered to remove sodium iodide. The filtrate was chromatographed on silica (Kieselgel 60; 200 g.) and the product was crystallised from ethanol to give 6-methoxy-2,4-bis(trichloromethyl)benzo[1,3]dioxin, m.p. 105°-107° C.

1. temperaturethe reaction mixture was warmed on a steam bath for 1 hour
2. customevaporated to dryness under reduced pressure
3. customthe oily residue was triturated with diethyl ether
4. filtrationfiltered
5. customto remove sodium iodide
6. customThe filtrate was chromatographed on silica (Kieselgel 60; 200 g.)
7. customthe product was crystallised from ethanol