Synthesis method of diclofenac sodium
A technology of diclofenac sodium and a synthesis method, which is applied in the field of medicinal chemistry, can solve the problems of high labor protection requirements for personnel, harsh reaction conditions, serious environmental pollution and the like, and achieves the effects of controlling synthesis cost, fewer reaction steps and good reaction effect.
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Embodiment 1
[0039] This embodiment comprises the following steps:
[0040] (1) Preparation of Diclofenac Methyl Ester
[0041] Methyl o-bromophenylacetate (4.6g, 0.02mol), 2,6-dichloroaniline (8.2g, 0.05mol), cuprous iodide (0.77g, 0.004mol), anhydrous potassium carbonate (5.6g, 0.04mol) and xylene (100ml) were placed in a dry reaction flask, under the protection of nitrogen, reflux reaction at 130°C for 40h under stirring, after the reaction was completed, activated carbon was added, suction filtered while hot, and the filtrate was concentrated to dryness under reduced pressure. The residue was dissolved in methanol, cooled and crystallized in an ice-water bath, filtered with suction, and dried to obtain 5.2 g of white solid (diclofenac methyl ester), with a yield of 83.1%. Melting point: 101-102°C, HPLC content greater than 98%.
[0042] (2) Synthesis of Diclofenac Sodium
[0043] Put sodium hydroxide (1.2g, 0.03mol) and methanol (40ml) in a reaction flask, add diclofenac methyl este...
Embodiment 2
[0046] This embodiment comprises the following steps:
[0047] (1) Preparation of Diclofenac Methyl Ester
[0048] Methyl o-bromophenylacetate (4.6g, 0.02mol), 2,6-dichloroaniline (9.8g, 0.06mol), cuprous iodide (0.96g, 0.005mol), anhydrous potassium carbonate (7.0g, 0.05mol) and xylene (100ml) were placed in a dry reaction flask, under the protection of nitrogen, reflux reaction at 140°C for 40h under stirring, after the reaction was completed, activated carbon was added, suction filtered while hot, and the filtrate was concentrated to dryness under reduced pressure. The residue was dissolved in methanol, cooled and crystallized in an ice-water bath, filtered with suction, and dried to obtain 5.4 g of white solid (diclofenac methyl ester), with a yield of 85.8%. Melting point: 101-102°C, HPLC content greater than 98%.
[0049] (2) Synthesis of Diclofenac Sodium
[0050] Sodium hydroxide (1.6g, 0.04mol) and methanol (40ml) were placed in a reaction flask, and diclofenac met...
Embodiment 3
[0053] This embodiment comprises the following steps:
[0054] (1) Preparation of Diclofenac Methyl Ester
[0055] Methyl o-bromophenylacetate (4.6g, 0.02mol), 2,6-dichloroaniline (8.2g, 0.05mol), copper powder (0.39g, 0.006mol), anhydrous potassium carbonate (8.4g, 0.06mol ) and N-methylpyrrolidone (100ml) were placed in a dry reaction flask, under the protection of nitrogen, reflux reaction at 120°C for 20h under stirring, after the reaction was completed, activated carbon was added, suction filtered while it was hot, and the filtrate was concentrated to dryness under reduced pressure. The residue was dissolved in methanol, cooled and crystallized in an ice-water bath, filtered with suction, and dried to obtain 5.1 g of white solid (diclofenac methyl ester), with a yield of 81.5%. Melting point: 101-102°C, HPLC content greater than 98%.
[0056] (2) Synthesis of Diclofenac Sodium
[0057] Put sodium hydroxide (2.0g, 0.05mol) and methanol (40ml) in a reaction flask, add di...
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