反应详情

温度

120 °C

83 g (0.6 mole) of potassium carbonate were added to a solution of 262 g (1.2 moles) of 7-chlorodibenzofuran-3-ol in 600 ml of dry dimethylformamide, and a solution of 212 g (2.55 moles) of ethylene carbonate in 300 ml of dimethylformamide was then added dropwise at 100° C. in the course of 90 minutes. The mixture was stirred at 120° C. for 8 hours and filtered off with suction at 100° C., and the filtrate was concentrated. The residue was dissolved in 2.5 l of ethyl acetate, the solution was washed three times with 300 ml of water each time, the organic layer was dried, decolorized with 10 g of animal charcoal and concentrated to 500 ml and the concentrate was cooled to 10° C. The precipitate was filtered off with suction and washed, at +5° C., with 60 ml of methanol, 50 ml of ether and 200 ml of petroleum ether in succession, and dried. 225 g of 2-(7-chlorodibenzofuran-3-oxy)-ethanol of melting point 118°-120° C. were obtained; yield: 71.4% of theory.

1. filtrationfiltered off with suction at 100° C.
2. concentrationthe filtrate was concentrated
3. dissolutionThe residue was dissolved in 2.5 l of ethyl acetate
4. washthe solution was washed three times with 300 ml of water each time
5. customthe organic layer was dried
6. concentrationconcentrated to 500 ml
7. temperaturethe concentrate was cooled to 10° C
8. filtrationThe precipitate was filtered off with suction
9. washwashed, at +5° C., with 60 ml of methanol, 50 ml of ether and 200 ml of petroleum ether in succession
10. customdried