Compound taking spirofluorene alkene structure as core, preparation method and applications thereof
A compound, spirofluorene technology, applied in chemical instruments and methods, organic chemistry, semiconductor/solid-state device manufacturing, etc., can solve different problems
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Embodiment 1
[0080] Embodiment 1: the synthesis of intermediate B1:
[0081]
[0082] In a 250ml three-neck flask, under the protection of nitrogen, add 0.01mol raw material 1-1, 0.012mol raw material 2-1, 150ml toluene and stir to mix, then add 5×10-5mol Pd 2 (dba) 3 , 5×10-5mol P(t-Bu) 3 , 0.03mol sodium tert-butoxide, heated to 105°C, refluxed for 24 hours, sampling plate, showed no bromide remaining, the reaction was complete; naturally cooled to room temperature, filtered, the filtrate was rotary evaporated to no fraction, passed through a neutral silica gel column , obtain target product intermediate B1; HPLC purity 99.37%, yield 73.4%; Elemental analysis structure (molecular formula C 24 h 19 N): theoretical value C, 89.68; H, 5.96; N, 4.36; tested value: C, 89.65; H, 5.99; N, 4.37. ESI-MS (m / z) (M+): The theoretical value is 321.42, and the measured value is 321.58.
Embodiment 2
[0083] Embodiment 2: the synthesis of intermediate C1:
[0084]
[0085] In a 250ml three-neck flask, under the protection of nitrogen, add 0.01mol of intermediate B16, 0.012mol of raw material 3-1, 150ml of toluene and stir to mix, then add 5×10 -5 mol Pd 2 (dba) 3 , 5×10 -5 mol P(t-Bu) 3 , 0.03mol sodium tert-butoxide, heated to 105°C, refluxed for 24 hours, sampling plate, showed no bromide remaining, the reaction was complete; naturally cooled to room temperature, filtered, the filtrate was rotary evaporated to no fraction, passed through a neutral silica gel column , to obtain the target product intermediate X1;
[0086] Under a nitrogen atmosphere, weigh 0.02mol of intermediate X1, 0.012mol of bis(pinacolate) diboron, 0.0002mol of Pd(dppf)Cl 2 1. Dissolve 0.05mol potassium acetate in toluene, react at 100-120°C for 12-24 hours, take a sample point plate, react completely, cool naturally, filter, and rotate the filtrate to obtain a crude product, pass through a ne...
Embodiment 3
[0092] Embodiment 3: the synthesis of compound 1:
[0093]
[0094] In a 250ml three-neck flask, under the protection of nitrogen, add 0.01mol raw material A1, 0.012mol intermediate B1, 150ml toluene and stir to mix, then add 5×10 -5 molPd 2 (dba) 3 , 5×10 -5 mol P(t-Bu) 3 , 0.03mol sodium tert-butoxide, heated to 105°C, refluxed for 24 hours, sampling plate, showed no bromide remaining, the reaction was complete; naturally cooled to room temperature, filtered, the filtrate was rotary evaporated to no fraction, passed through a neutral silica gel column , the target product was obtained, the HPLC purity was 99.63%, and the yield was 69.8%. Elemental analysis structure (molecular formula C 50 h 33 N): theoretical value: C, 92.70; H, 5.13; N, 2.16; test value C, 92.66; H, 5.22; N, 2.12. HPLC-MS: The molecular weight of the material is 647.82, and the measured molecular weight is 647.35.
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