Method for preparing adamantanemethanol from category A acid of adamantane
A technology of adamantane carboxyl ester and adamantane methanol is applied in the field of preparation of adamantane carbinol, and can solve the problems of severe reduction reaction, difficult control, high price and the like, and achieves low cost, simple and easy operation, and easy availability of raw materials. Effect
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Embodiment 1
[0011] Add 20 grams of adamantanecarboxylic acid and 100 ml of methanol into a 250 ml dry three-neck round bottom flask, and then add several zeolites. Heat to reflux in an oil bath at 70°C for 2-3 minutes to completely dissolve the solid. Then 5ml of concentrated sulfuric acid was added dropwise, and heated to reflux for 90min. Pour it into 500ml of water after cooling, neutralize it to weak alkalinity with sodium carbonate solution, precipitate solid, and suction filter to obtain 21.3 g of adamantane methyl carboxylate wet product, the purity of which is 99% according to GC analysis.
[0012] Then put 10 grams of the obtained wet product of methyl adamantane carboxylate, 30 ml of ethanol and 30 ml of tetrahydrofuran together into a round bottom flask and place it in a 74° C. oil bath for heating, stir with an electromagnetic stirrer until the solid is completely dissolved, and then Add 3.2 grams of NaBH every 30 minutes 4 and 4.2 g LiCl H 2 O was added into the flask in 8...
Embodiment 2
[0015] Add 20 grams of adamantanecarboxylic acid and 100 ml of ethanol to a 250 ml dry three-neck round bottom flask, and then add several zeolites. Heat to reflux in an oil bath for 2-3 minutes to completely dissolve the solid. Then 5ml of concentrated sulfuric acid was added dropwise, and heated to reflux for 90min. After cooling, it was poured into 500ml of water, neutralized to weak alkalinity with sodium carbonate solution, extracted three times with 50ml of ethyl acetate, and the combined organic layers were evaporated to remove the solvent to obtain 21.6g. The purity was 97% according to GC analysis.
[0016] Then put 10 grams of ethyl adamantane carboxylate, 30 ml of ethanol and 30 ml of tetrahydrofuran together into a round-bottomed flask and heat it in an oil bath at 74 ° C. Stir with an electromagnetic stirrer until the solid is completely dissolved, and then every 30 min 3.2 g NaBH 4 and 4.2 g LiCl H 2 O was added into the flask in 8 batches, heated and stirred ...
Embodiment 3
[0019] Add 20 grams of adamantanecarboxylic acid and 100 ml of methanol into a 250 ml dry three-neck round bottom flask, and then add several zeolites. Heat to reflux in an oil bath at 70°C for 2-3 minutes to completely dissolve the solid. Then 5ml of concentrated sulfuric acid was added dropwise, and heated to reflux for 90min. After cooling, pour it into 500ml of water, neutralize it to weak alkalinity with sodium carbonate solution, precipitate solid, and filter with suction to obtain 21.2 g of adamantane methyl carboxylate wet product, which has a purity of 99% according to GC analysis.
[0020] Put 10 grams of the obtained wet product of methyl adamantanecarboxylate and 60 ml of ethanol together into a round-bottomed flask and heat it in an oil bath. Stir with an electromagnetic stirrer until the solid is completely dissolved, and then mix 3.2 grams of it every 30 minutes. NaBH 4 and 4.2 g LiCl H 2 O was added into the flask in 8 batches, heated and stirred to react fo...
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