反应详情

温度

70 °C

1.95 g (80.2 mmol) of finely cut magnesium metal was placed in a 200 ml four-necked flask, and 50 ml of anhydrous tetrahydrofuran was further charged. The mixture was heated up to 70° C. while stirring, and 50 ml of a solution of 5 g (27.0 mmol) of 2-bromo p-xylene in anhydrous tetrahydrofuran was added dropwise while caring for steep reaction (reflux). After completion of the addition, it was refluxed for 30 minutes, then, cooled to 40° C., and to this was added 6.7 g (32.4 mmol) of dimethyloctylsilyl chloride while stirring. The solution was again heated and refluxed for 3 hours. The reaction mixture was charged in an aqueous saturated ammonium chloride solution, and extracted (toluene/water) and the organic phase was dried over sodium sulfate. After concentration, the product was purified and isolated by silica gel column chromatography (n-hexane) to obtain 3.19 g of 2-(dimethyloctylsilyl)-p-xylene.

1. customwhile caring for steep reaction (reflux)
2. additionAfter completion of the addition, it
3. temperaturewas refluxed for 30 minutes
4. temperaturecooled to 40° C.
5. stirringwhile stirring
6. temperatureThe solution was again heated
7. temperaturerefluxed for 3 hours
8. extractionextracted (toluene/water)
9. dry with materialthe organic phase was dried over sodium sulfate
10. concentrationAfter concentration
11. customthe product was purified
12. customisolated by silica gel column chromatography (n-hexane)