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ChemicalBook CAS DataBase List 2-Methacryloyloxy-2-methyladamantane
177080-67-0

2-Methacryloyloxy-2-methyladamantane synthesis

11synthesis methods
The synthesis of 2-Methyl-2-adamantylmethacrylate is as follows:Add 3546ml of n-heptane in the 5L four-necked flask equipped with stirring paddle, condenser tube and thermometer, turn on stirring, add 126.3g of 2-methyladamantanol to the system, and slowly add 0.022g polymerization inhibitor tetrachlorobenzoquinone to the reaction, add 110.8g basic ion exchange resin, adjust pH=7-8, cool down to -13°C, slowly add 110.8g vinyl methacrylate dropwise to the reaction system, keep the reaction for 7h, monitor the reaction progress, and take samples for detection After the reaction was completed, 1000 ml of water was added to the reaction system, and the mixture was stirred and extracted for phase separation. The organic phase was dried, concentrated under reduced pressure and evaporated to dryness to obtain 167 g of 2-methyl-2-adamantyl methacrylate product with a yield of 93.78%.

177080-67-0.png

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Yield:177080-67-0 93.78%

Reaction Conditions:

with 2,3,5,6-tetrachlorocyclohexa-2,5-diene-1,4-dione in n-heptane at -13; pH=7-8; for 7 h;Green chemistry;

Steps:

3 Example 3: Synthesis of 2-methyl-2-adamantyl methacrylate

Add 3546ml of n-heptane in the 5L four-necked flask equipped with stirring paddle, condenser tube and thermometer, turn on stirring, add 126.3g of 2-methyladamantanol to the system, and slowly add 0.022g polymerization inhibitor tetrachlorobenzoquinone to the reaction, add 110.8g basic ion exchange resin, adjust pH=7-8, cool down to -13°C, slowly add 110.8g vinyl methacrylate dropwise to the reaction system, keep the reaction for 7h, monitor the reaction progress, and take samples for detection After the reaction was completed, 1000 ml of water was added to the reaction system, and the mixture was stirred and extracted for phase separation. The organic phase was dried, concentrated under reduced pressure and evaporated to dryness to obtain 167 g of 2-methyl-2-adamantyl methacrylate product with a yield of 93.78%.Figure 3 shows the gas chromatogram of the 2-methyl-2-adamantyl methacrylate synthesized in this example.

References:

CN114560768,2022,A Location in patent:Paragraph 0065-0068; 0099

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