Synthetic method of imatinib
A kind of synthetic method, the technology of imatinib
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Embodiment 1
[0021] Under nitrogen protection, 10 mmol of 4-(3-pyridyl)-2-aminopyrimidine (CAS: 66521-66-2), 10 mmol of 4-chloromethylbenzoyl (3-bromo-4-methyl phenyl)amine (CAS: 1072105-05-5), 10 mmol of N-methylpiperazine (CAS: 109-01-3), 0.2 mmol of cuprous iodide, 0.2 mmol of N,N'- Diisopropylethylenediamine and 110 mmol of sodium acetate were dissolved in 20 mL of 1,4-dioxane, and the temperature of the reaction system was 100° C. for 4 hours to react.
[0022] After the reaction, the solvent was evaporated to dryness with a rotary evaporator, and the residue was separated by column chromatography to obtain 4.2 g of imatinib with a yield of 86%.
[0023] This reaction formula is as follows:
[0024]
Embodiment 2
[0026] Other conditions are the same as in Example 1, and the reactions of using different copper salts and their dosages are tested, and the experimental results are shown in Table 1.
[0027] Table 1 Test of different catalysts and their dosage effects
[0028] serial number Copper salt (amount mol / %) Yield(%) 1 Copper acetate (2) 56 2 Copper Bromide (2) 67 3 Copper Chloride (2) 70 4 Copper Sulfate (2) 55 5 Cuprous bromide (2) 78 6 Cuprous iodide (2) 86 (Example 1) 7 Cuprous iodide (1) 80 8 Cuprous iodide (3) 84 9 Cuprous iodide (4) 78 10 Cuprous iodide (5) 73
[0029] As can be seen from the above results, the use of 2 mol% cuprous iodide is the best, as in Example 1.
Embodiment 3
[0031] Other conditions are the same as in Example 1, and the reactions under different alkalis and different dosages thereof are checked, and the experimental results are as shown in Table 2.
[0032] Table 2 Test of different alkalis and their dosage effects
[0033] serial number Alkali (amount mol / %) Yield(%) 1 Sodium acetate (110) 86 (Example 1) 2 Sodium Carbonate (110) 64 3 Sodium Citrate (110) 60 4 Sodium acetate (100) 84 5 Sodium acetate (120) 80
[0034] From the above results, it can be seen that the effect of using 110 mol% sodium acetate is the best (Example 1).
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