反应详情

温度

90 °C

In an argon atmosphere, 225 g (1.58 mol) of diphosphorus pentaoxide was suspended in 320 mL of xylene, and 340 mL (256 g, 1.58 mol) of hexamethyldisiloxane was added thereto, followed by heating at 90° C. for about 1.5 hours. After the contents were almost dissolved, 90 g (316 mmol) of Compound A was added thereto, followed by heating at 160° C. for another 2 hours. After completion of the reaction, the reaction solution was cooled, and ice-water was added thereto. Then, the mixture was made alkaline by adding aqueous ammonia under cooling (inner temperature: 5° C. or lower), and was extracted with chloroform. After evaporation of the solvent, the residue was purified by silica gel column chromatography (hexane/ethyl acetate=1:1) to obtain 66.1 g of Compound B as a white solid (yield: 78%).

1. dissolutionAfter the contents were almost dissolved
2. temperatureby heating at 160° C. for another 2 hours
3. customAfter completion of the reaction
4. temperaturethe reaction solution was cooled
5. temperatureunder cooling (inner temperature: 5° C. or lower)
6. extractionwas extracted with chloroform
7. customAfter evaporation of the solvent
8. customthe residue was purified by silica gel column chromatography (hexane/ethyl acetate=1:1)