Process for producing 2-alkyl-2-adamantyl ester
A technology of adamantyl ester and adamantyl alkoxylithium, which is applied in the field of preparation of 2-alkyl-2-adamantyl ester, can solve the problems of difficult refining and low yield, and achieve simple refining and improved Yield, effect of simple preparation
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Embodiment 1
[0071] In a 500ml 4-neck flask equipped with a stirring blade, a thermometer, a condenser, and a dropping funnel, 30g of tetrahydrofuran and 2.78g (0.4mol) of lithium metal were added under a nitrogen atmosphere. In this solution, under a nitrogen atmosphere, the reaction temperature was controlled at about 40°C, and a solution of 30 g (0.2 mol) of 2-adamantanone (0.2 mol) and 26.2 g (0.24 mol) of ethyl bromide previously dissolved in 90 g of tetrahydrofuran was added dropwise. . After the dropwise addition, the temperature was raised to 45° C., and reaction aging was carried out for 1 hour.
[0072] After visually confirming the disappearance of metallic lithium, 4.36 g (0.04 mol) of ethyl bromide was added, followed by stirring at 45° C. for 1 hour to prepare a lithium 2-ethyl-2-adamantyl alkoxide solution. Analysis by gas chromatography (GC) confirmed that the conversion rate of 2-adamantanone at this time was 98%.
[0073] Replace the 500ml 4-neck flask with stirring bla...
Embodiment 2
[0077]In a 500ml 4-neck flask equipped with a stirring blade, a thermometer, a condenser, and a dropping funnel, 30g (0.2mol) of 2-adamantanone (0.2mol) and 26.2g (0.24mol) of ethyl bromide were dissolved in 120g of tetrahydrofuran under a nitrogen atmosphere. middle. Under a nitrogen atmosphere, the reaction temperature was controlled at about 40° C., and 2.78 g (0.4 mol) of lithium metal was added to the solution in five portions (0.5 g each time for the first four times, and 0.78 g for the last time). After the dropwise addition, the temperature was raised to 45° C., and reaction aging was carried out for 1 hour.
[0078] After visually confirming the disappearance of metallic lithium, 4.36 g (0.04 mol) of ethyl bromide was added, followed by stirring at 45° C. for 1 hour to prepare a lithium 2-ethyl-2-adamantyl alkoxide solution. Analysis by gas chromatography (GC) confirmed that the conversion rate of 2-adamantanone at this time was 93%.
[0079] Thereafter, the treatme...
Embodiment 3
[0082] According to the operation of Example 1, a solution of lithium 2-ethyl-2-adamantyl alkoxide was prepared. Analysis by gas chromatography (GC) confirmed that the conversion rate of 2-adamantanone at this time was 98%.
[0083] In the aforementioned solution obtained, 0.08 g (0.4 mmol) of phenothiazine was added as a polymerization inhibitor, and under a nitrogen atmosphere, the reaction temperature was cooled below 10° C., and 22.0 g (0.21 mol) of methacryloyl chloride was added dropwise thereto. ), and finished dripping in 2 hours. After completion of the dropwise addition, the mixture was stirred at 10° C. or lower for 4 hours to mature the reaction.
[0084] After reaction aging, 10 g of methanol and 16 g of a 10% by mass sodium hydroxide aqueous solution were added to the obtained reaction liquid while keeping the temperature below 10° C., and the organic layer was separated after stirring for 1 hour. After further washing the organic layer with a 10% by mass aqueo...
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