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A graphene-loaded fecl 3 Catalyst preparation method and its use in the preparation of anticancer drug intermediates
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A graphene and catalyst technology, which is applied in the preparation of anticancer drug intermediates and graphene-supported FeCl3 catalysts, can solve problems such as low product selectivity, iron-containing wastewater, and FeCl3 inability to separate, and achieves improved catalytic efficiency, conversion rate increase effect
Inactive Publication Date: 2017-12-01
孔令廷
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Problems solved by technology
[0008] 3-(2-Chloropyrimidin-4-yl)-1-methylindole needs a large amount of FeCl in the preparation process 3 , and generate a large amount of impurities, the selectivity of the product is low; and the later stage FeCl 3 It cannot be separated, and the amount of iron-containing wastewater in the post-treatment process is large, which brings huge environmental pressure;
[0009] Pan Tingting et al. (Chinese Journal of Pharmaceutical Industry, 2017, 48 (4): 483-487) on 1-methyl-1H-indole and FeCl 3 The feeding method has been improved, and the yield of the product has been improved; but the reaction still needs a large amount of FeCl 3 (equal molar amount with 2,4-dichloropyrimidine), and methanol and water crystallization were used in the purification process, resulting in a large amount of iron-containing wastewater
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Embodiment 1
[0034] Preparation of catalyst:
[0035] 100g powdered graphene oxide and 2g FeCl 3 Dissolve in 200ml of ethanol, stir for 30min; add 0.8g of ammonium nitrate and 0.6g of ammonium dihydrogen phosphate to the solution and stir for 30min; heat up to reflux for 30min, then distill off the ethanol to obtain a solid;
[0036] Put the solid in a calciner, heat up to 420-460°C at a rate of 3°C / min for calcination for 2-3 hours, then cool down to room temperature, and wash with ethanol and purified water;
[0037] After washing, dry at 90°C, and then crush to a particle size of less than 10 microns to obtain graphene-supported FeCl 3 catalyst.
Embodiment 2
[0039] Catalytic Preparation of 3-(2-Chloropyrimidin-4-yl)-1-methylindole
[0040] 1) Load 100g of 2,4-dichloropyrimidine and 20g of graphene prepared in Example 1 with FeCl 3 Put the catalyst in a mixed solution of ethanol and butanone (500ml, the volume ratio of ethanol and butanone is 4:1) and stir at 30-40°C for 20min;
[0041] 2) Lower the temperature of the reaction system to 15°C, then add 1-methyl-1H-indole in batches, and control the temperature of the reaction system not to exceed 15°C during the addition;
[0042] 3) After the addition of 1-methyl-1H-indole is completed, the temperature was raised to 30°C at a heating rate of 5°C / h, and the temperature was kept at 30°C for 3 hours; then the temperature was raised to 40°C at a heating rate of 5°C / h, and the ℃ heat preservation reaction for 2 hours; finally, the temperature was raised to 50 ℃ at a heating rate of 5 ℃ / h, and 50 ℃ heat preservation reaction was carried out for 1 hour;
[0043] 4) At the end of the hea...
Embodiment 3
[0051] Loading FeCl on recycled graphene 3 The catalyst was washed with ethanol and then dried. The results of recovery and application showed that the conversion rate of raw materials was 98.5%, and the selectivity of products was 95%. That is to say, there was basically no significant change in the activity of the catalyst, which could support recovery and application.
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Abstract
The invention belongs to the technical field of organic synthesis, and particularly relates to a preparation method for a graphene-supported FeC13 catalyst and application of the graphene-supported FeC13 catalyst to preparation of an anticancer drug intermediate. The preparation method comprises the following steps: modifying graphene by taking ammonium nitrate and ammonium dihydrogen phosphate as modifiers; meanwhile, supporting FeCl3 with the graphene to prepare the graphene-supported FeCl3 catalyst. The obtained catalyst is used for catalyzing to prepare the anticancer drug intermediate, namely, 3-(2-chloro-pyrimidine-4-yl)-1-methylindole, so that the raw material converting rate and product selectivity are improved greatly; moreover, the catalyst can be recycled, the production cost is lowered, and wastewater is not produced during production; an environment-friendly production process is provided.
Description
technical field [0001] The invention belongs to the technical field of organic synthesis, in particular to a graphene-loaded FeCl 3 The preparation method of the catalyst and its use in the preparation of anticancer drug intermediates. Background technique [0002] Osimertinib mesylate (osimertinib mesylate) chemical name N -[2-[(2-Dimethylaminoethyl)methylamino]-4-methoxy-5-[[4-(1-methylindol-3-yl)pyrimidin-2-yl] Amino]-phenyl]prop-2-enamide methanesulfonate, the structural formula is shown in (I) formula: [0003] [0004] (I) [0005] Osimertinib mesylate is a third-generation irreversible epidermal growth factor receptor tyrosine kinase inhibitor (EGFR-TKI) developed by AstraZeneca in the United Kingdom. It was approved for marketing by the FDA in November 2015. Its trade name is Tagrisso. Treatment of advanced non-small cell lung cancer with epidermal growth factor receptor (EGFR) T790M mutation or resistance to other EGFR inhibitors. [0006] 3-(2-Chloropyrimid...
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