(Trifluoromethyl)trimethylsilane synthesis
- Product Name:(Trifluoromethyl)trimethylsilane
- CAS Number:81290-20-2
- Molecular formula:C4H9F3Si
- Molecular Weight:142.2
Yield:81290-20-2 93.8%
Reaction Conditions:
with magnesium in tetrahydrofuran;ethylene dibromide at 0 - 30; for 2 h;Inert atmosphere;Solvent;
Steps:
1-7 Example 4
Dissolve 145.5g (1.34mol, 1.0eq) of trimethylchlorosilane in 500ml of THF to obtain solution A;Under the protection of nitrogen, add 500ml of THF to a 2L three-necked flask,38.6g (1.61mol, 1.2eq) of activated magnesium chips, and then 1mL 1,2-dibromoethane was added dropwise to the resulting system to be reacted to initiate,After the air bubbles are released from the system, the temperature of the system is reduced to 010,Then continue to feed bromotrifluoromethane gas into the reaction flask until the magnesium chips basically disappear (the process of feeding bromotrifluoromethane gas will heat up as the reaction progresses,When the temperature of the process control system is about 30°C, the amount of bromotrifluoromethane is about 200g (1.34mol, 1.0eq)).Then add the above solution A dropwise to it, and keep the reaction temperature at about 10°C, keep it for 2h after the dropwise addition is complete,Then add water to it for washing to dissolve all the solids, stand still and separate to obtain an organic phase, and separate the organic phase.Then water is added to the organic phase for washing, and after standing for stratification and separation, the final organic phase is distilled.After removing the solvent, the solid product obtained is the trifluoromethyltrimethylsilane product.The mass of trifluoromethyltrimethylsilane product is 178.7g, and the mass content of trifluoromethyltrimethylsilane is 99.6%.The yield of trifluoromethyltrimethylsilane product was 93.8%.
References:
CN113105492,2021,A Location in patent:Paragraph 0040-0063
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81290-20-2
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