Skeleton nickel catalyzed 5-nitrobenzimidazole ketone reducing process for preparing 5-aminobenzimidazole ketone
A technology for nitrobenzimidazolone and aminobenzimidazolone is applied in the field of preparation of 5-aminobenzimidazolone, can solve the problems of difficult recycling, environmental pollution, complicated post-treatment, etc., and achieves simple reaction operation and process. Simple, three wastes "less" effect
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[0008] Example 1 Add 30 g of nickel-aluminum alloy (binary) to a NaOH solution with a mass concentration of 19% and a volume of 200 ml, stir, the feeding temperature is 10-15° C., the feeding time is 2 hours, and then the temperature is raised to 20-25° C. , reacted for 9 hours, then used deionized water and absolute ethanol to filter and wash several times, and stored the obtained skeleton nickel in absolute ethanol for subsequent use, and marked it as W-1-(two) type.
[0009] Take 18g of 5-nitrobenzimidazolone, 80ml of absolute ethanol, and 1.8g of W-1-(two)-type skeleton nickel into the autoclave, feed hydrogen gas to a pressure of 2MPa, heat up to 85°C, and react for 6 hours. The catalyst was removed by liquid filtration, the filtrate was concentrated, filtered with suction, and the filter cake was dried in vacuum to obtain 14.0 g of 5-aminobenzimidazolone with a yield of 93.2%, a purity of 97.2%, and a melting point of 248-251°C.
[0010] Example 2 Add 40 g of nickel-alum...
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