Use of 1-methyl-4-isopropyl-bicyclo[2,2,2] octane-2,3-dicarboxylic acid
A technology of isopropyl and dicarboxylic acid, applied in welding medium, welding/cutting medium/material, organic chemistry, etc., can solve problems such as increased solder composition, complex structure of additives, complex composition, etc., and achieves less residue, Easy to wash, easy to synthesize
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Embodiment 1
[0014] Example 1 (preparation of 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-meng-3,8-diene 1.9%). After dripping, react at 135-140°C, remove the low boiling point components by distillation to obtain the crude product, and collect the lower fraction at 160-170°C / 3mmHg by distillation under reduced pressure to obtain the product 1-methyl-4-isopropyl-bicyclo[ 2,2,2]octene-2,3-dioic anhydride, the structure was determined by infrared spectroscopy and nuclear magnetic resonance.
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 a crude hydrogenated product, which was recrystallized with 2 ti...
Embodiment 3
[0018] Embodiment 3 (hydrolysis reaction)
[0019] Slowly add the hydrogenation product 1-methyl-4-isopropyl-bicyclo[2,2,2]octane-2,3-dioic anhydride obtained in Example 2 into an excess of 6M aqueous sodium hydroxide solution Stir, remove insolubles after extracting twice with methyl chloride, the aqueous solution layer is neutralized with 3N sulfuric acid aqueous solution, crystals are precipitated, and filtered under reduced pressure to obtain the white crystal hydrolysis product 1-methyl-4-isopropyl-bicyclo[ 2,2,2] Octane-2,3-dicarboxylic acid, mp 133.5-134.8°C, its structure determined by infrared spectroscopy and nuclear magnetic resonance, used as soldering agent A for soldering tests.
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