4-(三甲硅基)苯酚

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 8.32 g (0.05 mole) of p-trimethylsilylphenol was dissolved in 25 ml toluene. 6.1 g (0.06 mole) triethyl amine and 0.05 g hydroquinone was added. The solution was warmed. 5.43 g (0.06 mole) of acryloyl chloride was added over a 15 minute period. After 11/2 hours, the solution was washed two times with 5 percent sodium carbonate in water and separated. After washing with brine and separating, the organic phase was dried over magnesium sulfate, filtered, and the solvent removed in a rotary evaporator under reduced pressure. Vacuum distillation yielded 9.2 g of pure p-trimethylsilylphenyl acrylate. The solution was warmed After 11/2 hours, the solution was washed two times with 5 percent sodium carbonate in water separated After washing with brine separating the organic phase was dried over magnesium sulfate filtered the solvent removed in a rotary evaporator under reduced pressure Vacuum distillation

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 28.7 g p-trimethylsilylphenoxytrimethylsilane was dissolved in 9 ml 95 percent ethyl alcohol. One drop of concentrated hydrochloric acid and 4 ml water were added, and the mixture was shaked for 5 minutes. After standing for another 15 minutes, the mixture was washed two times with 30 ml water and separated. The organic phase was poured into a crystallizing dish; p-trimethylsilylphenol crystallized out as white needles. After drying overnight in vacuo, 18.7 g of product was obtained (mp 76 degrees Celsius). After standing for another 15 minutes the mixture was washed two times with 30 ml water separated The organic phase was poured into a crystallizing dish p-trimethylsilylphenol crystallized out as white needles After drying overnight in vacuo

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 8.32 g (0.05 mole) of p-trimethylsilylphenol was dissolved in 25 ml toluene. 6.1 g (0.06 mole) triethyl amine and 0.05 g hydroquinone was added. The solution was warmed. 5.43 g (0.06 mole) of acryloyl chloride was added over a 15 minute period. After 11/2 hours, the solution was washed two times with 5 percent sodium carbonate in water and separated. After washing with brine and separating, the organic phase was dried over magnesium sulfate, filtered, and the solvent removed in a rotary evaporator under reduced pressure. Vacuum distillation yielded 9.2 g of pure p-trimethylsilylphenyl acrylate. The solution was warmed After 11/2 hours, the solution was washed two times with 5 percent sodium carbonate in water separated After washing with brine separating the organic phase was dried over magnesium sulfate filtered the solvent removed in a rotary evaporator under reduced pressure Vacuum distillation

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 28.7 g p-trimethylsilylphenoxytrimethylsilane was dissolved in 9 ml 95 percent ethyl alcohol. One drop of concentrated hydrochloric acid and 4 ml water were added, and the mixture was shaked for 5 minutes. After standing for another 15 minutes, the mixture was washed two times with 30 ml water and separated. The organic phase was poured into a crystallizing dish; p-trimethylsilylphenol crystallized out as white needles. After drying overnight in vacuo, 18.7 g of product was obtained (mp 76 degrees Celsius). After standing for another 15 minutes the mixture was washed two times with 30 ml water separated The organic phase was poured into a crystallizing dish p-trimethylsilylphenol crystallized out as white needles After drying overnight in vacuo