反应详情

In a three-liter flask having four openings equipped with a stirrer, a thermometer, a dropping funnel, and a reflux condenser, respectively, 237 g (1.4 mol) of fluorene, 1 L of water, three drops of a surfactant, and five drops of sulfuric acid were placed and stirred to mix. By adding 230 g (1.4 mol) of bromine into the mixture, a reaction was started. After the reaction had been conducted at room temperature for 5 hours, unreacted bromine was decomposed with an aqueous solution of sodium hydrogen sulfite. The reaction product, which was a light yellow solid, was filtered and thus 334 g of a crude product was obtained. The crude product was dissolved in toluene and was subsequently washed with water and a sodium hydrogencarbonate aqueous solution. The resulting organic liquid was dried using anhydrous magnesium sulfate. After filtration, the liquid was concentrated and then allowed to stand at 0° C., so that a white solid was precipitated. The precipitate was filtered and subsequently washed with toluene, followed by drying. Thus, 287 g (1.1 mol, yield of 82%) of a white solid product was obtained. This product was subjected to gas chromatography and the purity of the product was 98.8%.

1. customequipped with a stirrer
2. additionto mix
3. filtrationwas filtered
4. customthus 334 g of a crude product was obtained
5. washwas subsequently washed with water
6. customThe resulting organic liquid was dried
7. filtrationAfter filtration
8. concentrationthe liquid was concentrated
9. customto stand at 0° C., so that a white solid
10. customwas precipitated
11. filtrationThe precipitate was filtered
12. washsubsequently washed with toluene
13. customby drying