A method for preparing 2-iodo-1-phosphoryl substituted alkanes by efficient difunctionalization of alkenes
A compound, phosphoryl technology, applied in the field of catalytic synthesis of organic phosphate compounds, can solve the problems of harsh reaction conditions, raw material quality and safety, product stability and purity, cross-substrate applicability, etc., to achieve the goal of reaction process Mild and easy to control, good industrial application prospects, simple and easy to implement effect
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Embodiment 1
[0025] 0.5 mmol of diphenylphosphoric acid, 1.0 mmol of styrene and 0.6 mmol of N - Iodosuccinimide (NIS) was added to the Schlenk tube under nitrogen atmosphere, and 1.0 mL of organic solvent (dichloromethane, dichloroethane, tetrahydrofuran, acetonitrile, toluene, N, N - dimethylformamide, dimethyl sulfoxide, methanol, ethanol, 1,4-dioxane, ethyl acetate), stirred and reacted at room temperature for 12 hours. Through GC detection and analysis, when tetrahydrofuran was used as the reaction solvent, the yield of the difunctionalization reaction was 66%.
Embodiment 2
[0027] 0.5 mmol of diphenylphosphoric acid, 1.0 mmol of styrene and 0.6 mmol of N -Iodosuccinimide was added to the Schlenk tube under nitrogen atmosphere, and 1.0 mL THF was added under nitrogen atmosphere, at the specified temperature (25 o C, 40 o C, 60 o C, 80 o C) The reaction was stirred for 12 hours. Analysis by GC detection at 40 o C, the yield of the difunctionalization reaction was 96%.
Embodiment 3
[0029] Mix 0.5 mmol of diphenylphosphoric acid, styrene (0.5 mmol, 0.6 mmol, 0.75 mmol, 1.0 mmol) with 0.6 mmol of N -Iodosuccinimide was added to the Schlenk tube under nitrogen atmosphere, and 1.0 mL THF was added under nitrogen atmosphere, at 40 o The reaction was stirred at C for 12 hours. By GC analysis, when the amount of styrene was 0.5 mmol, the yield of the difunctionalization reaction was 96%.
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