反应详情

A mixture of 98.4 g (0.45 mole) of 7-chlorodibenzofuran-3-ol, 200 ml of methyl ethyl ketone, 93 g (0.67 mole) of potassium carbonate and 283 g (1.4 moles) of dibromopropane was refluxed for 24 hours. The inorganic precipitate was filtered off with suction and the filtrate was concentrated under reduced pressure. The residue was dissolved in 500 ml of methylene chloride and the solution was washed with 100 ml of water, 100 ml of 2 N sodium hydroxide solution and 100 ml of water in succession, dried over sodium sulfate and concentrated under reduced pressure. The solid residue was left to stand with 30 ml of pentane at 0° C. for 30 minutes, filtered off with suction and washed with 30 ml of cold n-pentane. 77 g of pure 1-bromo-3-(7-chlorodibenzofuran-3-oxy)-propane of melting point 83°-85° C. were obtained; yield: 50% of theory.

1. temperaturewas refluxed for 24 hours
2. filtrationThe inorganic precipitate was filtered off with suction
3. concentrationthe filtrate was concentrated under reduced pressure
4. dissolutionThe residue was dissolved in 500 ml of methylene chloride
5. washthe solution was washed with 100 ml of water, 100 ml of 2 N sodium hydroxide solution and 100 ml of water in succession
6. dry with materialdried over sodium sulfate
7. concentrationconcentrated under reduced pressure
8. waitThe solid residue was left
9. filtrationfiltered off with suction
10. washwashed with 30 ml of cold n-pentane