BIS(PHENYLETHYNYL)DIMETHYLSILANE

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To 50 ml of tetrahydrofuran (THF) solution containing 6 ml of ethynylbenzene, 33 ml of 1.6N normal-butyl lithium was added dropwise under a nitrogen gas flow at 0° C. After stirring for 1 hour, 33.3 ml of THF solution containing 3 ml of dimethylsilyl chloride was added. After stirring at the room temperature for one night, the deposited solid was filtered and thereafter the obtained reaction solution was concentrated. Water was added to the solution, and then the solution was extracted with diethyl ether. Furthermore, the said diethyl ether layer was washed with water, thereafter dried with magnesium sulfate and concentrated. Then it was recrystallized from hexane, to obtain 5.02 g of bisphenylethynyldimethylsilane. was added dropwise under a nitrogen gas flow at 0° C was added After stirring at the room temperature for one night the deposited solid was filtered the obtained reaction solution was concentrated Water was added to the solution the solution was extracted with diethyl ether Furthermore, the said diethyl ether layer was washed with water dried with magnesium sulfate concentrated Then it was recrystallized from hexane

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To 50 ml of tetrahydrofuran (TBF) solution containing 6 ml of ethynylbenzene, 33 ml of 1.6N normal-butyl lithium was added dropwise under a nitrogen gas flow at 0° C. After stirring for 1 hour, 33.3 ml of THF solution containing 3ml of dimethylsilyl chloride was added. After stirring at the room temperature for one night, the deposited solid was filtered and thereafter the obtained reaction solution was concentrated. Water was added to the solution, and then the solution was extracted with diethyl ether. Furthermore, the said diethyl ether layer was washed with water, thereafter dried with magnesium sulfate and concentrated. Then it was recrystallized from hexane, to obtain 5.02 g of bisphenylethynyldimethylsilane. was added dropwise under a nitrogen gas flow at 0° C was added After stirring at the room temperature for one night the deposited solid was filtered the obtained reaction solution was concentrated Water was added to the solution the solution was extracted with diethyl ether Furthermore, the said diethyl ether layer was washed with water dried with magnesium sulfate concentrated Then it was recrystallized from hexane

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To 50 ml of tetrahydrofuran (THF) solution containing 6 ml of ethynylbenzene, 33 ml of 1.6N normal-butyl lithium was added dropwise under a nitrogen gas flow at 0° C. After stirring for 1 hour, 33.3 ml of THF solution containing 3 ml of dimethylsilyl chloride was added. After stirring at the room temperature for one night, the deposited solid was filtered and thereafter the obtained reaction solution was concentrated. Water was added to the solution, and then the solution was extracted with diethyl ether. Furthermore, the said diethyl ether layer was washed with water, thereafter dried with magnesium sulfate and concentrated. Then it was recrystallized from hexane, to obtain 5.02 g of bisphenylethynyldimethylsilane. was added dropwise under a nitrogen gas flow at 0° C was added After stirring at the room temperature for one night the deposited solid was filtered the obtained reaction solution was concentrated Water was added to the solution the solution was extracted with diethyl ether Furthermore, the said diethyl ether layer was washed with water dried with magnesium sulfate concentrated Then it was recrystallized from hexane