Preparation method of 1-phenyl adamantane and obtained 1-phenyl adamantane
A technology of phenyladamantane and adamantane, which is applied in the field of 1-phenyladamantane, can solve the problems of complex reaction and low yield, and achieve the effect of high reaction yield, low reaction temperature and green production process
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[0042] Example 1
[0043]Under nitrogen protection, add magnesium chips (2.64g, 0.11mol), 0.05g iodine, 100ml anhydrous tetrahydrofuran to a 500ml four-necked flask equipped with a mechanical stirrer, a reflux condenser, a constant pressure dropping funnel, and a thermometer, and heat to 60 degrees, add bromobenzene (15.7g, 0.1mol) dropwise, keep the solvent in a slightly boiling state, and obtain 0.1mol of bromobenzene Grignard reagent. Then continue to add dropwise 150ml tetrahydrofuran solution of 1-bromoadamantane (32.25g, 0.15mol), add anhydrous ferrous chloride (0.635g, 0.005mol), keep the temperature at 60 degrees and react for 24 hours, such as image 3 Shown is a schematic diagram of the reaction mechanism of ferrous chloride as a catalyst. TLC monitors the end of the reaction, cools to room temperature, adds a saturated aqueous ammonium chloride solution to quench the reaction, extracts the organic phase with ethyl acetate, and washes the organic phase with a saturat...
Example Embodiment
[0045] Example 2
[0046] Under nitrogen protection, add magnesium chips (2.64g, 0.11mol), 0.05g iodine, 100ml anhydrous ether to a 500ml four-necked flask equipped with a mechanical stirrer, a reflux condenser, a constant pressure dropping funnel, and a thermometer, and heat to 30 degrees, add bromobenzene (15.7g, 0.1mol) dropwise, keep the solvent in a slightly boiling state, and obtain 0.1mol of bromobenzene Grignard reagent. Then continue to drip 150ml ether solution of 1-bromoadamantane (32.25g, 0.15mol), add anhydrous ferrous chloride (0.635g, 0.005mol), keep the temperature at 35 degrees and react for 24 hours, such as image 3 Shown is a schematic diagram of the reaction mechanism of ferrous chloride as a catalyst. TLC monitors the end of the reaction, cools to room temperature, adds a saturated aqueous ammonium chloride solution to quench the reaction, extracts the organic phase with ethyl acetate, and washes the organic phase with a saturated aqueous sodium chloride ...
Example Embodiment
[0047] Example 3
[0048] Under nitrogen protection, add magnesium chips (2.64g, 0.11mol), 0.05g iodine, 100ml anhydrous tetrahydrofuran to a 500ml four-necked flask equipped with a mechanical stirrer, a reflux condenser, a constant pressure dropping funnel, and a thermometer, and heat to 60 degrees, add bromobenzene (15.7g, 0.1mol) dropwise, keep the solvent in a slightly boiling state, and obtain 0.1mol of bromobenzene Grignard reagent. Then continue to add dropwise 150ml tetrahydrofuran solution of 1-bromoadamantane (32.25g, 0.15mol), add cuprous chloride (0.99g, 0.01mol), keep the temperature at 60 degrees and react for 24 hours, such as Figure 4 Shown is a schematic diagram of the reaction mechanism of cuprous chloride as a catalyst. TLC monitors the end of the reaction, cools to room temperature, adds a saturated aqueous ammonium chloride solution to quench the reaction, extracts the organic phase with ethyl acetate, and washes the organic phase with a saturated aqueous...
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