A kind of synthetic method of 3-azidotrisilane
A technology of azidotrisilane and synthesis method, which is applied in the direction of silicon organic compounds, chemical instruments and methods, compounds of group 4/14 elements of the periodic table, etc., and can solve the cumbersome preparation and reactivity of 3-halotrisilane Inconsistency and other issues, to achieve the effect of easy operation, good functional group tolerance, and wide applicability
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[0027] General Procedure A: Synthesis of allyl azides. Its operation process is as follows:
[0028] To a stirred solution of HG-2 (2 mol%) in dichloromethane (1 mL / mmol) under argon was added alkene (1 eqiv) and allyl bromide (5 eqiv) dissolved in dichloromethane (2 mL / mmol) ) premixed solution and reacted at room temperature for 10 h. The dichloromethane solvent was removed to give crude allyl bromide. To the above solution of allyl bromide in anhydrous DMF (2 mL / mmol) and DMSO (1 mL / mmol) was added sodium azide (6eqiv) in portions and stirred at room temperature for 15h. After the reaction was completed, the resulting mixture was extracted with ethyl acetate and water, the aqueous layer was extracted three times, the combined organic layers were washed with saturated brine, the organic layer was dried over anhydrous sodium sulfate, filtered with suction and concentrated under reduced pressure. The corresponding allyl azide mixture was obtained by separation.
[0029] Th...
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