反应详情

温度

70 °C

25.0 g (137 mmol) of 4-ethylbiphenyl, 7.23 g (27.4 mmol) of orthoperiodic acid, 13.9 g (54.9 mmol) of iodine, 133 ml of acetic acid, 27 ml of water and 4.1 ml of sulfuric acid were placed in a 500 ml three-necked flask with a mechanical stirrer and bulb-shaped cooler. This was heated to 70° C. in a water bath, and subjected to the reaction for 2 hours. The product was cooled down to the ambient temperature. To this was added 300 ml of water, which was subjected to the extraction with chloroform. The resultant chloroform phase was washed with sodium thiosulfate and water in this order. To this was added sodium sulfate, and the dehydration was carried out. After the filtration was carried out, the chloroform was distilled away in an evaporator to obtain a light yellow solid. The resultant solid was recrystallized in the presence of ethanol to obtain a white crystal. The yield of the compound was 71%. Its melting point was 145-149° C. The IR chart is shown in FIG. 24.

1. customsubjected to the reaction for 2 hours
2. temperatureThe product was cooled down to the ambient temperature
3. extractionwas subjected to the extraction with chloroform
4. washThe resultant chloroform phase was washed with sodium thiosulfate and water in this order
5. additionTo this was added sodium sulfate
6. filtrationAfter the filtration
7. distillationthe chloroform was distilled away in an evaporator
8. customto obtain a light yellow solid
9. customThe resultant solid was recrystallized in the presence of ethanol
10. customto obtain a white crystal