Preparation method of adamantanols
A technology of adamantanol and adamantane, which is applied in the field of preparing adamantanols, can solve problems such as increased raw material costs and expensive catalysts, and achieve high yields
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Embodiment 1
[0050] 30 mL (582 mmol) of 25% by mass fuming sulfuric acid was added to a 100 mL four-necked flask, 2.4 g (58.5 mmol) of acetonitrile and 6.0 g (44.1 mmol) of adamantane were added, and the mixture was reacted at a reaction temperature of 25° C. for 3 hours. It should be noted that the molar ratio of oleum to the raw material adamantane was 13.2 (=582 / 44.1).
[0051] Next, the reaction liquid was added dropwise to 90 g of water at 70° C. charged in a 4 L four-necked flask. When the dropwise addition was completed, the temperature of the mixed liquid of water and the reaction liquid was 75°C. After the dropwise addition was completed, the hydrolysis was completed by stirring at 80° C. for 30 minutes. After cooling to room temperature, the precipitated crystals were filtered and dried to obtain 6.6 g of crystals.
[0052] According to gas chromatography analysis, the crystals were 1-adamantanol with a GC purity of 99.6%, and the yield was 98%.
Embodiment 2
[0054] Except having adjusted the addition amount of acetonitrile to 3.6 g (87.7 mmol), the same operation as Example 1 was performed. As a result, 6.5 g of 1-adamantanol with a GC purity of 99.7% was obtained, and the yield was 97%.
Embodiment 3
[0056] Except having made reaction temperature into 40 degreeC, the same operation as Example 1 was performed. As a result, 6.2 g of 1-adamantanol with a GC purity of 97.6% was obtained, and the yield was 92%.
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