1,1,3,3-Tetramethyl-disiloxane → 1,1,3,3-Tetramethyl-1-[1-(trimethoxysilyl)ethyl]disiloxane
Reaction equation
[CH3:1][SiH:2]([CH3:7])[O:3][SiH:4]([CH3:6])[CH3:5].[CH:8]([Si:10]([O:15][CH3:16])([O:13][CH3:14])[O:11][CH3:12])=[CH2:9]>>[CH3:12][O:11][Si:10]([O:15][CH3:16])([O:13][CH3:14])[CH:8]([Si:2]([CH3:7])([CH3:1])[O:3][SiH:4]([CH3:6])[CH3:5])[CH3:9]Participants
Conditions
- Temperature
- 65 °C
Procedure
A four-necked flask equipped with a reflux condenser, stirrer, addition funnel and thermometer was thoroughly purged with nitrogen. In the nitrogen blanket, the flask was charged with 134.3 g (1 mol) of 1,1,3,3-tetramethyldisiloxane and 0.026 g (0.1 mmol) of RhCl3.3H2O to form a mixture. The mixture was heated to 60-70° C. and maintained at the temperature. With stirring, 148.2 g (1 mol, equimolar to 1,1,3,3-tetramethyldisiloxane) of vinyltrimethoxysilane was added dropwise to the mixture from the addition funnel over 6 to 7 hours. After the completion of dropwise addition, the reaction mixture was maintained at 60-70° C. and aged for 1 to 2 hours, driving the reaction to completion. On vacuum distillation, a product having a boiling point of 92-95° C. at 1.3 kPa was collected. The 1-(trimethoxysilyl)ethyl-1,1,3,3-tetramethyldisiloxane product was obtained in a yield of 93%. On gas chromatography analysis, the product was identified to be a mixture of two isomers, alpha-adduct:
Workup
- customA four-necked flask equipped with a reflux condenser, stirrer, addition funnel
- customthermometer was thoroughly purged with nitrogen
- customto form a mixture
- temperaturemaintained at the temperature
- additionAfter the completion of dropwise addition
- temperaturethe reaction mixture was maintained at 60-70° C. and aged for 1 to 2 hours
- customthe reaction to completion
- distillationOn vacuum distillation
- customwas collected
Sources & evidence
- ORD record
- ord-bf0c6972f356425f83ad6d183c015d26
- Source dataset
- uspto-grants-2007_10
- Patent number
- US07279589B2
Reaction notes
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