Synthesis of maleimidotriethoxy silane-series compounds, and preparation method of self-assembled film
A technology of maleimidotriethoxysilane and its synthesis method, which is applied in the fields of chemical instruments and methods, compounds of Group 4/14 elements of the periodic table, organic chemistry, etc., and can solve the problem of catalytic yield and repeatability Poor and other issues
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Embodiment 1
[0026] (1) Synthesis of self-assembly material 11-maleimidoundecyltriethoxysilane.
[0027]
[0028] Synthesis of 10-undecylenamide:
[0029]
[0030] Take urea (15g, 0.25mol) and undecylenic acid (23.01g, 0.125mol) in a two-necked flask, raise the temperature to 170-180°C, and stop heating after 4 hours of reaction. When the temperature drops to 110-120°C, add 5% Na 2 CO 3 The solution (100-150ml) was used to stop the reaction, and the mixture was placed in an ice-water bath, filtered after solid precipitation, recrystallized twice with 95% ethanol, and vacuum-dried to obtain a colorless solid with a yield of 60%. 1 HNMR (400MHz; CDCl 3 ): δ5.80 (1H, m), 5.47 (2H, s), 2.22 (2H, t), 2.04 (2H, m), 1.63 (2H, m), 1.38-1.29 (10H, m).
[0031] Synthesis of 11-amino-1-undecene:
[0032]
[0033] Take LiAlH 4 (2.3g, 60.6mmol), 50ml of dry THF in a 250ml two-necked flask, protected by nitrogen, heated to reflux for 30min and then stopped heating. Compound 10-undecylena...
Embodiment 2
[0041] (1) Preparation of self-assembled membrane
[0042] Step 1: Wash the silicon wafer with a size of 1cm×1cm with a neutral detergent and wash it with a large amount of ultrapure water;
[0043] Step 2: Sonicate silicon wafers with acetone, ethanol, and ultrapure water for 10 minutes in sequence and use N 2 blow dry;
[0044] Step 3: Incorporate the cleaned Si / SiO 2 The substrate is immersed in the piranha solution (H 2 SO 4(conc.) / H 2 o 2(30%) =5:1) for 24h to form hydroxyl groups on its surface;
[0045] Step 4: Dip the activated silicon wafer in 10ml of toluene (dry) solution of 11-maleimidoundecyltriethoxysilane (10 -3 M), N 2 protected, heated to 75°C, and self-assembled for 48h, the Si / SiO 2 A self-assembled film of 11-maleimido undecyltriethoxysilane is self-assembled on a substrate.
[0046] (2) Characterization of materials
[0047] (a) X-ray photoelectron spectroscopy (XPS)
[0048] figure 2 It is the XPS schematic diagram of N1s. The peak with bin...
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