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Production methods of Climbazole CAS 38083-17-9

03-17-2022

1. A preparation method of high-purity climbazole (CAS 38083-17-9), comprising the following steps: reacting 200-320 parts by mass of toluene, 100 parts of Chloroether ketone, 30-70 parts of imidazole and 5-12 parts of acid binding agent under 100-ihtc for 3-5 hours; Primary crystallization: after the reaction, add 80 ~ 100 parts by mass of water, wash at 50 ~ 60 ° C, stand for water separation, then lower the temperature to 30 ~ 35 ° C, distill and crystallize under reduced pressure, and separate the crude gambolin; Recrystallization: put 100 parts by mass of crude gamboline into 200 ~ 400 parts by mass of toluene, raise the temperature to 80 ~ 90 ° C, fully dissolve, add 1 ~ 3 parts by mass of activated carbon for pressure filtration, cool to 30 ~ 35 ° C for crystallization after pressure filtration, and then centrifuge to obtain high-quality gamboline, and dry the refined gamboline at 65 ~ 79 ° C.



2. The preparation method of high-purity gamboline according to claim 1, which is characterized in that in the recrystallization step, when the crude gamboline is fully dissolved in toluene, 30wt.% is added first Wash with 5-10 parts by mass of liquid alkali, then add 120-300 parts by mass of water for water washing, and then press filtration and crystallization after water separation.

3. The preparation method of high-purity gamboline according to claim 1 or 2, which is characterized in that the acid binding agent is n, n-dimethylbenzylamide.