反応 #53765

反応方程式

fluorenone

sodium hydrogen sulfite

bromine

bromine

water

→

yellow solid

収率 92.9%

2-bromofluorenone

収率 92.9%

溶媒

toluene

反応条件

後処理

1. 1
   その他equipped with a stirrer
2. 2
   workup.ADDITIONto mix
3. 3
   ろ過was filtered
4. 4
   その他thus 365 g of a crude product was obtained
5. 5
   洗浄was subsequently washed with water
6. 6
   その他The resulting organic liquid was dried
7. 7
   ろ過After filtration
8. 8
   濃縮the liquid was concentrated
9. 9
   その他to stand at 0° C., so that a yellow solid
10. 10
    その他was precipitated
11. 11
    ろ過The precipitate was filtered
12. 12
    洗浄subsequently washed with toluene
13. 13
    その他by drying

実験手順

In a three-liter flask having four openings equipped with a stirrer, a thermometer, a dropping funnel, and a reflux condenser, respectively, 256 g (1.4 mol) of fluorenone, 1 L of water, three drops of a surfactant, and five drops of sulfuric acid were placed and stirred to mix. By adding 250 g (1.6 mol) of bromine into the mixture, a reaction was started. After the reaction had been conducted at 50° C. for 12 hours, unreacted bromine was decomposed with an aqueous solution of sodium hydrogen sulfite. The reaction product, which was a dark yellow solid, was filtered and thus 365 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 yellow solid was precipitated. The precipitate was filtered and subsequently washed with toluene, followed by drying. Thus, 339 g (1.3 mol, yield of 92%) of a yellow solid product was obtained. This product was subjected to gas chromatography and the purity of the product was 99.4%.

出典