Preparation method of deferasirox derivative

A technology of derivatives and products, applied in the field of medicine, can solve the problems of complex synthetic routes of deferasirox derivatives, difficult purification and purification, low total synthesis yield, etc., achieves convenient purification, low production cost, and overcomes separation and purification. cumbersome effect

Active Publication Date: 2014-02-05
TLC NANJING PHARMA RANDD CO LTD
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  • Abstract
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Problems solved by technology

[0003] In the prior art, the synthesis route of deferasirox derivatives is relatively complicated, mainly because the total synthesis yield is very l

Method used

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  • Preparation method of deferasirox derivative

Examples

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Effect test

Embodiment 1

[0024] Example 1 Preparation of Derasirox Derivatives

[0025] like figure 1 Shown:

[0026] (1) Dissolve methyl salicylate (0.046mol) in dry dimethylformamide solvent (56ml), add potassium hydroxide (0.185mol) at low temperature, then add benzyl chloride (0.046mol) dropwise, After the reaction was stirred at room temperature for 4 hours, 100ml of water was added. After the reaction mixture was stirred for 1 hour, the pH was adjusted to 1 with acid in an ice bath, extracted with ethyl acetate (200mlx3), and the organic phase was dried with anhydrous sodium sulfate and evaporated. Drying yielded 8.5 g of white solid intermediate 1 (benzylsalicylic acid); used directly in the next reaction.

[0027] (2) Suspend 8.5 g of intermediate product 1 prepared in step (1) in 21 ml of thionyl chloride, reflux for 4 hours, and evaporate to dryness to obtain 7.5 g of oil. Compound 2, (2-(2-hydroxyphenyl)-4H-1,3-benzoxazin-4-one) (0.023mol) was suspended in 57ml of dry dichloromethane and...

Embodiment 2

[0033] The deferasirox derivative prepared in Example 1 of the present invention was used in 100 patients with iron overload caused by blood transfusion. Experiments showed that the effective rate was 100%, and no adverse reactions were observed.

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Abstract

The invention discloses a preparation method of a deferasirox derivative. The preparation process comprising optimal reactant usage amount, reaction temperatures, reaction time, reaction steps and the like is determined via a large quantity of experimental screening. The whole preparation process is strong in maneuverability, high in preparation efficiency and low in production cost; and especially, the total yield can reach more than 30%. Compared with the prior art that the total yield is only 14% or so, the preparation process disclosed by the invention has a good technical effect. In addition, the whole preparation process is convenient for purification, thereby overcoming the technical defect of complicated separation and purification in the prior art and having the relatively high production efficiency. Thus, the industrial mass production can be realized.

Description

technical field [0001] The invention relates to a preparation method of a compound, in particular to a preparation method of deferasirox derivatives, belonging to the technical field of medicine. Background technique [0002] Deerasirox, the chemical name is 4-[3,5-bis(2-hydroxyphenyl)-1,2,4-triazol-1-yl]benzoic acid, is a ferric drug researched and developed by Swiss Novartis pharmaceutical company The chelating agent product was approved by the FDA in November 2005. Iron chelators are currently the only effective treatment for transfusion-induced iron overload. Deerasirox is a once-daily oral iron chelator indicated for the treatment of iron overload from blood transfusions in patients 2 years of age and older with chronic anemia. [0003] In the prior art, the synthesis route of deferasirox derivatives is relatively complicated, mainly because the total synthesis yield is very low, only about 14%, and in the preparation process, the purification is difficult, the proced...

Claims

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Application Information

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IPC IPC(8): C07D249/08A61P7/00
CPCC07D249/08
Inventor 马富孙春峰王忠义刘春
Owner TLC NANJING PHARMA RANDD CO LTD
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