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ChemicalBook CAS DataBase List 1,3-Dichloro-1,1,3,3-tetraisopropyldisiloxane
69304-37-6

1,3-Dichloro-1,1,3,3-tetraisopropyldisiloxane synthesis

2synthesis methods
can be prepared starting from trichlorosilane by treatment with i-PrMgCl, H2O, and acetyl chloride. Alternatively, it can be prepared by the reaction of 1,1,3,3- tetraisopropyldisiloxane with CCl4 in the presence of catalytic PdCl2.This method is also suitable for its in situ preparation.
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Yield:69304-37-6 87%

Reaction Conditions:

with trichloroisocyanuric acid in tetrahydrofuran at -20; for 0.25 h;Inert atmosphere;Schlenk technique;

Steps:

Chlorination procedure 3 for complete chlorination
General procedure: Chlorination where all Si-H bonds had to be chlorinated were performed in THF, TCCA was used in excess (1 eq. TCCA / 1 eq.siloxane). A flask was filled with educt and THF and cooled down to -20°C (20 mlTHF/g educt). TCCA was added in small portions, under intense stirring. After TCCAa ddition was completed, stirring was continued for 15 minutes, afterwards, the cooling bath was removed and the solution was allowed to come to room temperature. Varying siloxane chain lengths, substituents or Si-H bond positions affected the method in whichcompounds were isolated and characterized. THF and unreacted TCCA had to be removed soon after the reactions were completed, otherwise product degeneration was observed after a few days.

References:

Hafner, Thomas;Torvisco, Ana;Uhlig, Frank [Journal of Organometallic Chemistry,2018,vol. 875,p. 1 - 4] Location in patent:supporting information

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