Directly-thermocurable organic siloxane, manufacture method and application
A technology for curing products and reactions, applied in chemical instruments and methods, organic chemistry, organic insulators, etc., can solve the problems of difficult to control pre-polymerization, high cost of aryne resin synthesis, and large heat release.
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Embodiment 14
[0127] The preparation of embodiment 14-(methylpropargyloxy)-1-bromobenzene
[0128]
[0129] Under argon protection, add 51.9 grams of 4-bromo-phenol (0.3mol), 66.5 grams of methyl bromide propyne (0.5mol) and 300 milliliters of DMSO (dimethyl sulfoxide) steamed now in the reaction device, room temperature After stirring for 30 minutes, 53 grams of anhydrous sodium carbonate (0.5mol) was added. After reacting at room temperature for 10 hours, the reaction mixture solution was poured into water, stirred vigorously for 20 minutes, and the product was extracted with chloroform in batches. After washing with sodium chloride aqueous solution, chloroform was removed by rotary evaporation, and the obtained solid was washed with water and a small amount of ethanol to obtain 60 g of the product, with a yield of 89%. Hydrogen spectrum characterization ( 1 H NMR, 300MHz, CDCl 3 )7.55(d,2H),6.70(d,2H)4.55(s,2H),0.39(s,3H)
Embodiment 24
[0130] The preparation of embodiment 24-(methylpropargyloxy)-1-bromobenzene
[0131]
[0132] Under argon protection, add 51.9 grams of 4-bromo-phenol (0.3mol), 45.5 grams of methyl chloride propyne (0.5mol) and 300 milliliters of DMSO (dimethyl sulfoxide) steamed now in the reaction device, room temperature After stirring for 30 minutes, 53 grams of anhydrous sodium carbonate (0.5mol) was added. After reacting at room temperature for 10 hours, the reaction mixture solution was poured into water, stirred vigorously for 20 minutes, and the product was extracted with chloroform in batches. After washing with sodium chloride aqueous solution, chloroform was removed by rotary evaporation, and the obtained solid was washed with water and a small amount of ethanol to obtain 55 g of the product, with a yield of 81.5%. Hydrogen spectrum characterization ( 1 H NMR, 300MHz, CDCl 3 )7.55(d,2H),6.70(d,2H),4.55(s,2H),0.39(s,3H).
Embodiment 34
[0133] The preparation of embodiment 34-(methylpropargyloxy)-1-chlorobenzene
[0134]
[0135] Under argon protection, add 38.7 grams of 4-chloro-phenol (0.3mol), 66.5 grams of methyl bromide propyne (0.5mol) and 300 milliliters of DMSO (dimethyl sulfoxide) steamed now in the reaction apparatus, room temperature After stirring for 30 minutes, 53 grams of anhydrous sodium carbonate (0.5mol) was added. After reacting at room temperature for 10 hours, the reaction mixture solution was poured into water, stirred vigorously for 20 minutes, and the product was extracted with chloroform in batches. After washing with sodium chloride aqueous solution, chloroform was removed by rotary evaporation, and the obtained solid was washed with water and a small amount of ethanol to obtain 45 g of the product, with a yield of 82.9%. Hydrogen spectrum characterization ( 1 H NMR, 300MHz, CDCl 3 ) 7.55 (d, 2H), 6.70 (d, 2H), 4.55 (s, 2H), 0.36 (s, 3H).
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