Preparation method of 3, 5-dimethyl-4-chlorophenol
A technology of dimethylphenol and chlorophenol, which is applied in the preparation of organic compounds, chemical instruments and methods, organic chemistry and other directions, can solve the problems of increasing the difficulty of post-processing, and achieve the improvement of the conversion rate of the substrate, the simple process flow, and the reduction of The effect of pollution
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Embodiment 1
[0030] The preparation method of embodiment 1,3,5-dimethyl-4-chlorophenol
[0031] Add 122g of 3,5-dimethylphenol (1mol) into a 1000ml three-necked flask, then add 366g of glacial acetic acid, start stirring, start to add 141.8g of sulfuryl chloride (1.05mol) dropwise at 25°C, and control the reaction temperature at 30-35°C ℃, drop time 3h; after the drop is completed, the reaction is terminated, the sample is analyzed by GC, and the results are MX: 0.35%, PCMX: 90.5%, OCMX: 7.4%, DCMX: 1.75%.
[0032] The material was distilled under reduced pressure to remove the solvent glacial acetic acid, and then purified by rectification (control the vacuum degree -0.09Mpa, the kettle temperature was 150°C, and the fraction with a top temperature of 130°C was collected), and 138g of white crystal product was obtained. The GC analysis result was, MX: 0.10%, PCMX: 99.6%, OCMX: 0.22%, DCMX: 0.08%. The yield was 88.1% (molar yield based on MX).
Embodiment 2
[0033] The preparation method of embodiment 2,3,5-dimethyl-4-chlorophenol
[0034] Add 122g of 3,5-dimethylphenol (1mol) into a 1000ml three-necked flask, then add 488g of glacial acetic acid, start stirring, start adding 148.5g of sulfuryl chloride (1.1mol) dropwise at 20°C, and control the reaction temperature at 20-25°C , the dropping time was 4h; after the dropping was completed, the reaction was terminated, and the samples were analyzed by GC, and the results were MX: 0.15%, PCMX: 87.5%, OCMX: 8.4%, and DCMX: 3.95%.
[0035] The material was distilled under reduced pressure to remove the solvent glacial acetic acid, and then purified by rectification to obtain 130 g of a white crystal product. The GC analysis results were: MX: 0.07%, PCMX: 99.43%, OCMX: 0.32%, DCMX: 0.18%. The yield was 83.0% (molar yield based on MX).
Embodiment 3
[0036] The preparation method of embodiment 3,3,5-dimethyl-4-chlorophenol
[0037] Add 122g of 3,5-dimethylphenol (1mol) into a 1000ml three-necked flask, then add 366g of formic acid, start stirring, start to drop 145.8g of sulfuryl chloride (1.08mol) at 20°C, control the reaction temperature at 30-40°C, The dropping time was 2 hours; after the dropping was completed, the reaction was terminated, and the samples were analyzed by GC, and the results were MX: 0.45%, PCMX: 85.52%, OCMX: 11.35%, and DCMX: 2.68%.
[0038] The material was purified by rectification after vacuum distillation to remove the solvent formic acid to obtain 128g of white crystal product. GC analysis results were: MX: 0.15%, PCMX: 99.22%, OCMX: 0.39%, DCMX: 0.24%. The yield was 81.7% (molar yield based on MX).
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