Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | 1-Hexanol | HCID 8103 | — |
| Reactant | Trifluoromethanesulfonic acid | HCID 62406 | — |
| Reactant | 1,3-Disiloxanediol, 1,1,3,3-tetramethyl- | HCID 70697 | — |
| Reactant | 1,8-Diazabicyclo(5.4.0)undec-7-ene | HCID 81184 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | HCID 22506159 | HCID 22506159 | — |
Reaction Steps
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.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06875880B2 |
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| Source dataset | uspto-grants-2005_04 |
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| ORD ID | ord-440be0f6a7844653a8b021f55c53d372 |
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| Source note | uspto-grants-2005_04 |
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