Use of 1-methyl-4-isopropyl-bicyclo[2, 2, 2] octane-2, 3-diacid anhydride
A technology of isopropyl and dianhydride, which is applied to 1-methyl-4-isopropyl-bicyclo[2, can solve the problems of increased solder composition, complex composition, limited use, etc., and achieves low soldering temperature, High welding activity, low cost effect
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[0012] The specific preparation method is: using α-terpinene and maleic anhydride as starting materials, using intermolecular Diels-Alder (Diels-Alder) cycloaddition reaction to first synthesize 1-methyl-4-iso Propyl-bicyclo[2,2,2]octene-2,3-dioic anhydride is then hydrogenated. The hydrogenation reaction conditions are; use 5% Pd / C as a catalyst, and its consumption is 1-10% of the raw material weight, the pressure of hydrogen is at 0.1-1.0MPa, use such as methanol, ethanol and other alcohols as solvents, and the consumption is The weight is 2-20 times, the hydrogenation reaction temperature is carried out under the condition of 20-35 ℃, and the content of the target substance is controlled by gas chromatography analysis. After the hydrogenation reaction, the catalyst and solvent are removed to obtain the target composition, and the target compound with higher purity can be obtained by recrystallization. In addition, as the main active ingredient, its structural feature is a...
Embodiment 1
[0014] Embodiment 1 (preparation of raw material 1-methyl-4-isopropyl-bicyclo[2,2,2]octene-2,3-dioic anhydride)
[0015] In a four-necked flask equipped with a thermometer, a dropping funnel, a mechanical stirrer, and a condenser tube, add maleic anhydride (calculated as 2.5 times moles based on α-terpinene) and heat to dissolve the maleic anhydride, which is controlled at 65 At -70°C, drop the terpinene mixture from the dropping funnel (α-terpinene oil content 32.4%, γ-terpinene 15.6%, iso-terpinene 14.6%, isoterpinene 6.9%, Dipentene 5.1%, camphene 4.5%, β-pinene 3.5%, α-pinene 3.4%, p-Mentha-3,8-diene (p-Mentha-3.8-diene) 1.9%). After dripping, react at 135-140 degrees for 6 hours, carry out quantitative analysis, and use α-terpinene as the limiting reagent to calculate the yield to be 168.6%. The cycloaddition product 1-methyl-4-isopropyl-bicyclo[2,2,2]octene-2,3- dianhydride.
Embodiment 2
[0016] Embodiment 2 (hydrogenation reaction)
[0017] 20g of the distillation product 1-methyl-4-isopropyl-bicyclo[2,2,2]octene-2,3-dioic anhydride synthesized in Example 1 was dissolved in 50ml of methanol, and the methanol solution Place it in an autoclave, then weigh 1.0 g of Raney nickel catalyst (Raney NiW2), wash it with methanol until neutral, and add it to the reaction kettle. After replacing the air in the kettle with hydrogen, fill the hydrogen to 3MPa, start the stirrer at 100°C, adjust the stirring speed to 500rpm, the reaction starts, the reactants begin to absorb hydrogen, and the hydrogen pressure drops. When the hydrogen pressure dropped to 0.1MPa, the hydrogen was replenished to 3MPa, and this operation was repeated, and the reaction was completed after 40 hours. After the catalyst was removed under reduced pressure with a filter aid, the solvent was evaporated with a rotary evaporator to obtain the target composition with a main active ingredient content of ...
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