反应 #1576338
相关文献 (1)
openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US06875880B2
反应条件: temp:35.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: A 100-ml four-necked flask equipped with a Dimroth condenser, stirrer and thermometer was thoroughly purged with nitrogen and then charged with 60 ml of toluene, 0.075 g (5.0×10−4 mol) of trifluoromethanesulfonic acid, 0.076 g (5.0×10−4 mol) of 1,8-diazabicyclo[5.4.0]-7-undecene, and 5.1 g (5.0×10−2 mol) of 1-hexanol, which were stirred. Further, 4.15 g (2.5×10−2 mol) of 1,1,3,3-tetramethyldisiloxane-1,3-diol was admitted into the reactor, which was evacuated to a reduced pressure of 4.7 kPa and heated at 35° C. The reactor was kept at the temperature for two hours and resumed atmospheric pressure. Composition analysis by gas chromatography revealed that 1,1,3,3-tetramethyldisiloxane-1,3-diol had completely reacted, and 1,3-dihexyloxy-1,1,3,3-tetramethyldisiloxane was produced at a selectivity of 79.1%. By-products included 1,5-dihexyloxy-1,1,3,3,5,5-hexamethyltrisiloxane and 1,7-dihexyloxy-1,1,3,3,5,5,7,7-octamethyltetrasiloxane. A 100-ml four-necked flask equipped with a Dimroth condenser, stirrer and thermometer was thoroughly purged with nitrogen was evacuated to a reduced pressure of 4.7 kPa had completely reacted
来源 ID: ord-440be0f6a7844653a8b021f55c53d372