Preparation method and device of 2-isopropyl-2-adamantanol (meth)acrylate
A technology of acrylate and adamantanol, applied in the field of preparation of 2-isopropyl-2-adamantanol (meth)acrylate, can solve problems such as large pollution and equipment corrosion, achieve complete reaction and save production Cost, simple effect of purification process
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Embodiment 1
[0038] Embodiment one: the preparation of isopropyl adamantyl methacrylate
[0039] See attached figure 1 , is a schematic diagram of the device structure used in this embodiment.
[0040] The device comprises a first reactor 1 and a second reactor 3, and the outlet pipeline of the first reactor 1 is connected to the second reactor 3 through a plate filter 2 with a pore size of 1 micron; a collection tank 4 is provided, and the second The mother liquid separated in the reaction kettle 3 is transported to the collection tank 4 through the collection pipeline; the first reaction kettle 1 and the second reaction kettle 3 are respectively provided with agitators 5 .
[0041] The preparation process can be expressed by the following formula:
[0042]
[0043] See attached figure 2 , is a schematic flow chart of the preparation method of this embodiment. Specifically:
[0044] Weigh 120g (1.2mol) of methyl methacrylate, 194g (1mol) of isopropyl adamantanol, 3.4g (0.02mol) o...
Embodiment 2
[0046] Embodiment two: the preparation of isopropyl adamantane methacrylate
[0047]
[0048] Weigh 250g (2.2mol) of ethyl methacrylate, 388g (2mol) of isopropyl adamantanol, 9.3g (0.03mol) of sodium methoxide catalyst, and 1440g (20mol) of tetrahydrofuran into a 10L reactor, and set the reaction temperature to 77°C , Stop the reaction after 24 hours, filter the reaction solution with a 1 micron plate filter at 77°C, and collect the sodium methoxide catalyst for later use.
[0049] Introduce the filtrate into the reaction kettle, turn on the freezer and stir, set the temperature at -20°C, and precipitate a large amount of solids after about 5 hours, stop stirring, let it stand for 1 hour, insert a catheter into the reaction kettle, and vacuum the liquid out, and the solid product Take it out, put it in a vacuum drying oven, and dry it at 25°C for 24 hours. The collected product weighs 513g, the yield is 98.0%, and the purity is 99.5% (HPLC). 1 H NMR (400M, C 6 D. 6 ) : δ=5...
Embodiment 3
[0050] Embodiment three: the preparation of isopropyl adamantane acrylate
[0051]
[0052] Weigh 103g (1.2mol) of methyl acrylate, 194g (1mol) of isopropyl adamantanol, 6.2g (0.02mol) of sodium methoxide catalyst, and 880g (10mol) of dichloromethane into a 5L reactor, set the reaction temperature to 77°C After 24 hours, stop the reaction, filter the reaction solution with a 1 micron plate filter at 77°C, collect the sodium methoxide catalyst and leave it for later use, introduce the filtrate into the reaction kettle, turn on the refrigerator and stir, and set the temperature to -30°C After about 2 hours, a large amount of solids were precipitated. Stop stirring, let stand for 1 hour, insert a catheter into the reaction kettle, vacuumize the liquid, take out the solid product, put it in a vacuum drying oven, and dry it at 25°C for 24 hours to collect the product. Weighing 251g, yield 95.8%, purity 99.2% (HPLC), NMR results 1 H NMR (400M, C 6 D. 6 ) : δ=5.660(1H), 6.438(1...
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