Preparation method of 1-bromine naphthalene
A technology of bromonaphthalene and bromine water, which is applied in the field of catalytic synthesis of 1-bromonaphthalene, can solve the problems of environmental pollution, high cost of raw materials, difficulty in recycling, etc., and achieve an environmentally friendly effect
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Embodiment 1
[0019] The first step, put 0.4mmol naphthalene and 0.2560g OMImBr ionic liquid into a closed reactor, add 0.5120g glacial acetic acid and stir and mix evenly, then add saturated bromine water containing 0.2mmol bromine simple substance;
[0020] The second step is to seal the airtight reactor treated in the first step and place it in a water bath with a temperature of 20°C for constant temperature reaction for 3 hours, take out the airtight reactor, open it after natural cooling, and extract it with benzene;
[0021] The third step is to add toluene reference substance in the solution obtained after benzene treatment, and carry out gas chromatographic analysis. The yield can reach more than 95% (calculated by naphthalene).
[0022] In the fourth step, the bottom liquid left after the extraction is taken and reused, and the yield of the target product can reach more than 80% (calculated by naphthalene).
Embodiment 2
[0024] The first step, put 0.4mmol naphthalene and 0.5120gBMImPF6 ionic liquid into a closed reactor, add 0.5120g glacial acetic acid and stir and mix evenly, then add saturated bromine water containing 0.3mmol elemental bromine;
[0025] The second step is to seal the airtight reactor treated in the first step and place it in a water bath with a temperature of 40°C for constant temperature reaction for 6 hours, take out the airtight reactor, open it after natural cooling, and extract it with acetone;
[0026] The 3rd step, in the solution gained after acetone treatment, add toluene standard substance, carry out gas chromatographic analysis. The yield can reach more than 95% (calculated by naphthalene).
[0027] In the fourth step, the bottom liquid left after the extraction is taken and reused, and the yield of the target product can reach more than 80% (calculated by naphthalene).
Embodiment 3
[0029] The first step, 0.4mmol naphthalene and 0.7680g OMImPF6 ionic liquid are put into airtight reactor, add 2.5600g glacial acetic acid simultaneously and mix well, then add the saturated bromine water of 0.4mmol elemental bromine;
[0030] The second step is to seal the airtight reactor treated in the first step and place it in a water bath with a temperature of 50°C for a constant temperature reaction for 24 hours, take out the airtight reactor, open it after natural cooling, and extract it with petroleum ether;
[0031] The third step, adding toluene reference substance in the solution obtained after petroleum ether treatment, carries out gas chromatographic analysis. The yield can reach more than 95% (calculated by naphthalene).
[0032] In the fourth step, the bottom liquid left after the extraction is taken and reused, and the yield of the target product can reach more than 80% (calculated by naphthalene).
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