Strong nucleophilic organic phosphine compound for polymerization of polar vinyl monomer, preparation method and application thereof
A vinyl monomer, strong nucleophilic technology, applied in the fields of periodic table group 5/15 element compounds, organic chemistry, chemical instruments and methods, etc., to achieve mild polymerization conditions, convenient operation, and high catalytic activity.
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Embodiment 1
[0034]
[0035] The synthesis of the raw material functionalized bisimidazole functionalized organic guanidine (BIG-1) can be found in the literature (Angew. Chem. Int. Ed., 2014, 53, 1435-1438). In a glove box, BIG-1 (0.48 mmol), diisopropylphosphine chloride (0.48 mmol), and tetrahydrofuran (3 mL) were added to a 50 mL Schlenk bottle containing a magnetron, respectively. After the reaction was stirred at 25°C for 24 hours, the tetrahydrofuran was removed in vacuo, and the precipitated solid was washed with n-hexane (3×10 mL) to obtain the target product precursor salt intermediate BIG-1-HCl.
[0036] Intermediate BIG-1-HCl (0.45 mmol), potassium hydride (0.68 mmol), potassium tert-butoxide (0.045 mmol) and tetrahydrofuran (5 mL) were added to a 25 mL round bottom flask, respectively. After the reaction was stirred at 25°C for 2 hours, the solid was removed by suction filtration, and the solvent was removed in vacuo to obtain the target product BIG-1-P. Yield was 85%.
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Embodiment 2
[0040]
[0041] In a glove box, BIG-2 (0.48 mmol), di-tert-butylphosphine chloride (0.48 mmol), and tetrahydrofuran (3 mL) were added to a 20-mL Schlenk bottle containing a magnetron, respectively. After the reaction was stirred at 25°C for 24 hours, the tetrahydrofuran was removed in vacuo, and the precipitated solid was washed with n-hexane (3×10 mL) to obtain the target product precursor salt intermediate BIG-2-HCl.
[0042] The intermediate (0.45 mmol), potassium hydride (0.68 mmol) were respectively )、 Potassium tert-butoxide (0.045 mmol) and tetrahydrofuran (5 mL) were added to a 25 mL round bottom flask. After the reaction was stirred at 25°C for 2 hours, the solid was removed by suction filtration, and the solvent was removed in vacuo to obtain the target product BIG-2-P. The yield was 87%.
[0043]
[0044] Dark red solid. 1 H NMR (400MHz, C 6 D 6 )δ4.93(dt,J=13.9,6.9Hz,4H),1.68(s,12H),1.56(d,J=9.7Hz,18H),1.40(d,J=7.1Hz,25H). 13 C NMR (151MHz, C 6 D 6 )δ...
Embodiment 3
[0046]
[0047] In a glove box, BIG-3 (0.48 mmol), dicyclohexylphosphine chloride (0.48 mmol), and tetrahydrofuran (3 mL) were added to a 20 mL Schlenk bottle containing a magnetron, respectively. After the reaction was stirred at 25°C for 24 hours, the tetrahydrofuran was removed in vacuo, and the precipitated solid was washed with n-hexane (3×10 mL) to obtain the target product precursor salt intermediate BIG-3-HCl.
[0048] Intermediate (0.45 mmol), potassium hydride (0.68 mmol), potassium tert-butoxide (0.045 mmol) and tetrahydrofuran (5 mL) were added to a 25 mL round bottom flask, respectively. After the reaction was stirred at 25°C for 2 hours, the solid was removed by suction filtration, and the solvent was removed in vacuo to obtain the target product BIG-3-P. Yield was 65%.
[0049]
[0050] Yellow solid. 1 H NMR (400MHz, C 6 D 6 )δ4.95(dt,J=13.7,6.7Hz,4H),2.31(dd,J=40.0,12.3Hz,5H),2.03-1.75(m,13H),1.67(d,J=4.8Hz,12H) ),1.42(d,J=7.0Hz,25H),1.09(s,2H). 13 ...
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