Synthesis process of methotrexate
A methotrexate and synthetic process technology, which is applied in the field of pharmaceutical compounds, can solve problems such as complex operation process, difficult to obtain raw materials, and high requirements for reaction conditions, and achieve the effects of simple process operation, short production cycle, and high purity
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Embodiment 1
[0045] The synthetic technique of embodiment 1 methotrexate
[0046] 1) Synthesis of crude methotrexate
[0047] Synthesis method: Take 250ml of distilled water, 39g of L-p-aminobenzoyl glutamic acid zinc salt, 9.6g of 2,4,5,6-tetraaminopyrimidine sulfate, put them into a flask, adjust with 12mol / L concentrated hydrochloric acid The pH of the solution is 2-3, add 36ml of ethanol, 12g of 1,1,3-tribromoacetone, reflux reaction at 25°C, after the reaction lasts for 2 hours, add 2g of sodium acetate trihydrate to it, and continue the reaction for 24 hours to obtain Crude methotrexate.
[0048] synthetic route:
[0049]
[0050] 2) refining the synthetic methotrexate crude product into pure methotrexate
[0051] Synthesis method: put the synthesized methotrexate yellow solid in a round bottom flask, add 100ml of distilled water into it, the solid part dissolves, then adjust the pH to 10-11 with 40% NaOH solution, the yellow solid gradually dissolves until the solution turns r...
Embodiment 2
[0054] The synthetic technique of embodiment 2 methotrexate
[0055] 1) Synthesis of crude methotrexate
[0056] Synthesis method: Take 200ml of distilled water, 30g of L-p-aminobenzoyl glutamic acid zinc salt, 8g of 2,4,5,6-tetraaminopyrimidine sulfate, put them into a flask, adjust the solution with 12mol / L concentrated hydrochloric acid PH to 2-3, add 30ml of ethanol, 8g of 1,1,3-tribromoacetone, reflux reaction at 20°C, after the reaction lasts for 1 hour, add 1g of sodium acetate trihydrate to it, and continue the reaction for 20 hours to obtain formazan Crude aminopterin;
[0057] synthetic route:
[0058]
[0059] 2) refining the synthetic methotrexate crude product into pure methotrexate
[0060] Put the synthesized yellow solid methotrexate in a round-bottomed flask, add 100ml of distilled water into it, the solid part dissolves, then adjust the pH to 10-11 with 35% NaOH solution, the yellow solid gradually dissolves until the solution is reddish brown and clear...
Embodiment 3
[0063] The synthetic technique of embodiment 3 methotrexate
[0064] 1) Synthesis of crude methotrexate
[0065] Synthesis method: Take 300ml of distilled water, 50g of L-p-aminobenzoyl glutamic acid zinc salt, 11g of 2,4,5,6-tetraaminopyrimidine sulfate, put them into a flask, adjust the solution with 12mol / L concentrated hydrochloric acid PH to 2-3, add 42ml of ethanol, 16g of 1,1,3-tribromoacetone, condense and reflux reaction at 30°C, after the reaction lasts for 4 hours, add 4g of sodium acetate trihydrate to it, and continue the reaction for 28 hours to obtain formazan Crude aminopterin;
[0066] synthetic route:
[0067]
[0068] Refining synthetic crude methotrexate into pure methotrexate
[0069]Put the synthesized yellow solid of methotrexate in a round bottom flask, add 100ml of distilled water into it, the solid is partially dissolved, then adjust the pH to 10-11 with 45% NaOH solution, the yellow solid gradually dissolves until the solution is reddish brown ...
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