Hydrogenation calalyst of N-(3,4-dimethyl phenyl amine)-D-riboside
A xylidine and catalyst technology, applied in the field of modified Raney nickel catalyst, can solve the problems of target product ribosamine purity analysis, high cost, low catalyst activity, etc., and achieve simple preparation process, excellent product quality and strong selectivity Effect
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Embodiment 1
[0019] Add 9 grams of metal nickel, 9 grams of metal aluminum and 0.54 grams of metal molybdenum in the graphite crucible, put it into the electric arc furnace, first vacuumize it to 1Pa at 573K, and then fill the furnace with argon to 6×10 4 Pa, melt at high temperature, stir evenly, and cool to get nickel-aluminum-transition metal multi-element alloy.
[0020] Add 74ml of 28% NaOH solution in the flask, then add 15g of pulverized nickel-aluminum-transition metal multi-element alloy, react at 90°C for 2 hours, remove the supernatant by pouring, and wash with water until neutral.
[0021] The prepared modified Raney catalyst was stored in pure water for later use.
[0022] 3.4g 3,4-dimethylaniline is dissolved in 15ml ethanol, is transferred in the autoclave, then adds the Raney catalyst (wet weight, the same below) of 3.0g transition metal modification, 15mg boric acid, according to the inventor in CN00135818 55ml of D-ribose ethanol solution (containing 3.975g of D-ribose) ...
Embodiment 2
[0028] The method is the same as in Example 1, except that the amount of the transition metal-modified Raney nickel catalyst is changed to 2.0 g, and other conditions remain unchanged. 6.0 g of crude ribosamine was obtained, the purity by HPLC method was 99.4%, and the crude yield and pure yield of ribosamine were 88.9% and 88.4% respectively.
Embodiment 3
[0032] The method is the same as in Example 1, the amount of transition metal-modified Raney nickel catalyst is 4.0g, D-ribose is used instead of the method purification provided by the inventor in CN 00135818.9, and the glucose fermentation using the current domestic semi-synthetic riboflavin production The D-ribose ethanol solution 53ml (containing ribose 3.975g) of the 7.5g / 100ml concentration obtained by liquid extraction process, other conditions are all unchanged, obtains ribosamine crude product 5.4g, HPLC method purity 98.4%, ribosamine crude product yield, folded The pure yields were 80.0%, 78.7%, respectively.
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