Method for preparing quaternary phosphonium salt compounds
A technology of compound and quaternary phosphonium salt, which is applied in the field of preparation of quaternary phosphonium salt compounds, can solve the problems of high toxicity and insufficient variety of quaternary phosphonium salt compounds, and achieve the effects of low cost, simple method and simple device
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Embodiment 1
[0036] Embodiment one: see attached figure 1 , a preparation method of a quaternary phosphonium salt compound, comprising the following steps:
[0037] (1) 0.05 mmol of cuprous iodide (CuI), 0.05 mmol of iodine (I 2 ), 0.05 mmol 1,4-bis(diphenylphosphine)butane (C 28 h 28 P 2 ) and 1 milliliter of methanol are reaction starters, mixed in 1 milliliter of acetonitrile, and reacted for 70 hours under solvothermal reaction conditions;
[0038] (2) Then slowly lower the temperature to obtain a colorless solution. The solution was concentrated by diffusion with two volumes of diethyl ether to obtain colorless rod-like crystals. Its single crystal structure (C 30 h 34 P 2 ) (Cu 2 I 4 )like figure 1 As shown, the methyl group on methanol is transferred to the P of 1,4-bis(diphenylphosphine)butane to form the cation of quaternary phosphonium salt (C 30 h 34 P 2 ) 2+ , the anion is (Cu 2 I 4 ) 2- dimer.
[0039] (3) The crystalline product was enriched by filtration, ...
Embodiment 2
[0043] Embodiment two: see attached figure 2 , a preparation method of a quaternary phosphonium salt compound, comprising the following steps:
[0044] (1) 0.05 mmol of cuprous iodide (CuI), 0.05 mmol of iodine (I 2 ), 0.05 mmol 1,4-bis(diphenylphosphine)butane (C 28 h 28 P 2 ) and 0.15 gram of benzyl alcohol are reaction initiators, mixed in 2 milliliters of acetonitrile, and reacted for 70 hours under solvothermal reaction conditions;
[0045] (2) Then slowly lower the temperature to obtain a colorless solution. The solution was naturally evaporated and concentrated at room temperature to obtain colorless blocky crystals. Its single crystal structure (C 42 h 42 P 2 ) (Cu 2 I 4 )like figure 2 As shown, the benzyl group on the benzyl alcohol is transferred to the P of 1,4-bis(diphenylphosphine)butane to form the cation of the quaternary phosphonium salt (C 42 h 42 P 2 ) 2+ , the anion is (Cu 2 I 4 ) 2- dimer.
[0046] (3) The crystalline product is enriche...
Embodiment 3
[0050] Embodiment three: see attached image 3 , a preparation method of a quaternary phosphonium salt compound, comprising the following steps:
[0051] (1) Add 0.05 mmol of mercury iodide (HgI), 0.05 mmol of iodine (I 2 ), 0.05 mmol 1,4-bis(diphenylphosphine)butane (C 28 h 28 P 2 ) and 0.15 gram of benzyl alcohol are reaction initiators, mixed in 2 milliliters of acetonitrile, and reacted for 70 hours under solvothermal reaction conditions;
[0052] (2) Then slowly lower the temperature to obtain a colorless solution. The solution was naturally evaporated and concentrated at room temperature to obtain colorless blocky crystals. Its single crystal structure (C 42 h 42 P 2 ) (Hg 2 I 6 )like image 3 As shown, the benzyl group on the benzyl alcohol is transferred to the P of 1,4-bis(diphenylphosphine)butane to form the cation of the quaternary phosphonium salt (C 42 h 42 P 2 ) 2+ , the anion is (Hg 2 I 6 ) 2- dimer.
[0053] (3) The crystalline product is enr...
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