Synthetic process of phosphorus ligand type compound
A synthesis process and compound technology, which is applied in the field of synthesis process of phosphorus ligand compounds, can solve the problems of low yield and cumbersome synthesis operation, and achieve the effect of simple operation process and significant application value
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[0015] Example 1
[0016] This embodiment relates to a synthesis process of phosphorus ligand compounds, including the following steps:
[0017] Step 1: Dissolve 1-bromopropane and triphenylphosphine in dichloromethane in equal moles (both are 1 mole), stir evenly, then add acetic acid to adjust and maintain the pH of the reaction system at 1.7, and then increase the temperature Perform reflux reaction at 35°C for 16 hours, then adjust the pH of the reaction system to 3.5 with sodium hydride;
[0018] Step two, cooling to 5°C, after crystallization is complete, filter to obtain a filter cake;
[0019] In step three, the filter cake was washed with dichloromethane and dried in vacuum to obtain 362.8 g of a white solid, namely (1-propyl)triphenylphosphonium bromide, with an HPLC purity of 99.4% and a yield of 93.6%.
[0020] 1 H-NMR(CDCl 3 , 500MHz)δ: 0.87(t, CH 3 ), 1.65(m,CH 2 ), 3.74(t,CH 2 -P + ), 7.74 (s, benzene ring hydrogen).
Example Embodiment
[0021] Example 2
[0022] This embodiment relates to a synthesis process of phosphorus ligand compounds, including the following steps:
[0023] Step 1: Dissolve 1-bromopropane and triphenylphosphine in dichloromethane in equal moles (both are 1 mole), stir evenly, then add acetic acid to adjust and maintain the pH of the reaction system at 1.2, and then increase the temperature Perform reflux reaction at 38°C for 20 hours, then adjust the pH of the reaction system to 3.8 with sodium hydride;
[0024] Step two, cooling to 1°C, after crystallization is complete, filter to obtain a filter cake;
[0025] Step 3: Wash the filter cake with dichloromethane, and obtain 358.9 g of off-white solid after vacuum drying, namely (1-propyl)triphenylphosphonium bromide, with an HPLC purity of 99.2% and a yield of 92.4%.
[0026] 1 H-NMR(CDCl 3 , 500MHz) δ: 0.88 (t, CH 3 ), 1.64(m,CH 2 ), 3.75(t,CH 2 -P + ), 7.76 (s, benzene ring hydrogen).
Example Embodiment
[0027] Example 3
[0028] This embodiment relates to a synthesis process of phosphorus ligand compounds, including the following steps:
[0029] Step 1: Dissolve 1-bromopropane and triphenylphosphine in dichloromethane in equal moles (both are 1 mole), stir evenly, then add acetic acid to adjust and maintain the pH of the reaction system at 2.0, and then increase the temperature Perform reflux reaction at 40°C for 13 hours, then adjust the pH of the reaction system to 3.2 with sodium hydride;
[0030] Step 2: Cool to 3°C, filter after crystallization is complete, to obtain a filter cake;
[0031] In step three, the filter cake was washed with dichloromethane, and 356.1 g of off-white solid was obtained after vacuum drying, namely (1-propyl)triphenylphosphonium bromide, with an HPLC purity of 99.1% and a yield of 91.6%.
[0032] 1 H-NMR(CDCl 3 , 500MHz)δ: 0.87(t, CH 3 ), 1.66(m,CH 2 ), 3.73(t,CH 2 -P + ), 7.73 (s, benzene ring hydrogen).
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