A kind of preparation method of medicine intermediate for treating type Ⅱ diabetes
A precursor, methyluracil technology, applied in the field of preparation of drug intermediates for the treatment of type 2 diabetes, to achieve the effects of avoiding side reactions, low cost, and high catalytic performance
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Embodiment 1
[0036] Prepare the palladium metal catalyst modified by ammonium metatungstate, comprising the following steps:
[0037] 1) At room temperature, add 20g of nano-silicon nitride to 200ml of aqueous solution for ultrasonic dispersion, and then add 1.2g of PdCl 2 .2H 2 Two mixtures of O and ammonium metatungstate (PdCl in the mixture 2 .2H 2 O and ammonium metatungstate molar ratio is 1:0.4) stirred to obtain the first mixed solution;
[0038] 2) The temperature of the first mixed solution was raised to 50°C, and the ammonia solution was added dropwise to adjust the pH to 9.5-10.5, and kept stirring for 3-5 hours to obtain the second mixed solution;
[0039] 3) Suction filtration, drying the filter cake at 80-100°C under a nitrogen atmosphere, and then calcining at 200-240°C for 2 hours to obtain a catalyst precursor;
[0040] 4) The catalyst precursor was reduced in a hydrogen atmosphere at 350-380°C for 2 hours to obtain a palladium metal catalyst modified by ammonium metatun...
Embodiment 2
[0046] Using the preparation method of Example 1, respectively with nanoscale Al 2 o 3 、TiO 2 or ZrO 2 Replace nano-silicon nitride as a carrier (but the added weight of each carrier is consistent with the weight of nano-silicon nitride) to prepare ammonium metatungstate-modified palladium metal catalysts with different supports, namely Cat / Al 2 o 3 、Cat / TiO 2 or Cat / ZrO 2 ;
[0047] Using 6-amino-5-nitroso-1-methyluracil as the substrate, the catalysts prepared by using the above-mentioned different supports were used to evaluate the catalytic performance. -5-Nitroso-1-methyluracil 10g is placed in 100ml ethanol, feeds hydrogen and carries out hydrogenation reaction at room temperature and normal pressure, HPLC detects the reaction solution situation after 2h, and the result is as shown in table 2:
[0048] The catalytic effect of catalyst prepared by different supports in table 2
[0049] catalyst
Conversion rates / %
Selective / %
Embodiment 1 pr...
Embodiment 3
[0056] Reduction at different temperatures in the catalyst preparation process results in a large difference in the morphology of the catalysts, specifically manifested as differences in the specific surface area, pore volume, and pore diameter of the catalyst, thereby affecting the catalytic performance of the catalyst; the present invention has systematically studied the catalyst preparation process in the early stage. Influence of the reduction temperature in step 4) on the catalytic reaction (the reaction conditions are: respectively take 0.5 g of the catalyst obtained at different reduction temperatures and 10 g of the substrate 6-amino-5-nitroso-1-methyluracil in 100 ml In ethanol, hydrogenation was carried out at room temperature and normal pressure by introducing hydrogen, and the reaction liquid was detected by HPLC after 2 hours), the results are shown in Table 3 below:
[0057] Table 3 Catalytic properties of catalysts prepared at different reduction temperatures
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