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ChemicalBook CAS DataBase List tert-Butyldimethylsilyl chloride
18162-48-6

tert-Butyldimethylsilyl chloride synthesis

15synthesis methods
tert-butyldimethylsilyl chloride (TBSCI) was synthesized by the reaction of tert-butyllithium with dichlorodimethylsilane.
The pentane solution of dichlorodimethylsilane was cooled to 0°C, and the pentane solution of tert-butyllithium was added dropwise with stirring under nitrogen. The temperature was maintained at 0 °C, stirred for 1.5 h and then heated to 25 °C, and the reaction was continued for 48 h. Distillation, collect 125 ℃ (97.5kPa) fractions, stand to solidify, and obtain tert-butyldimethylsilyl chloride. Yield 70%.
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Yield:18162-48-6 99.8%

Reaction Conditions:

palladium diacetate

Steps:

7 Example 7

Example 7 To a 500 ml glass flask equipped with a stirring machine, a thermometer, a reflux condenser and a dropping funnel, there were added 135.8 g (1.5 mole) of methallyl chloride and 0.05 g of palladium acetate, the temperature of the mixture was raised up to 60 to 70° C., then 116.3 g (1.0 mole) of t-butyldimethylsilane was dropwise added to the mixture over 3 hours through the dropping funnel to carry out the reaction of the methallyl chloride and the t-butyldimethylsilane and the reaction mixture was aged at 100° C. for 2 hours. The reaction solution obtained after the aging was distilled to give a distillate having a boiling point range of from 124 to 126° C. Thus, 145.9 g of t-butyldimethylchlorosilane having a purity of 99.8% was obtained. The yield of the product was found to be 96.8%.

References:

US5342984,1994,A

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