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Preparation technology o high-purity gefitinib

A gefitinib and preparation process technology, applied in the field of pharmaceutical compound preparation, can solve the problems of many types of solvents, long production cycle, many steps, etc., and achieve the effects of high purity, reduced production cost, and reduced types

Active Publication Date: 2012-07-18
REYOUNG PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This reaction route has the disadvantages of many types of solvents used, large amount, many steps, long production cycle, high energy consumption, and low purity.

Method used

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  • Preparation technology o high-purity gefitinib

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] The preparation technology of high-purity gefitinib of the present invention is as follows:

[0036] 1: Add 10g 7-methoxy-6-(3-morpholin-4-ylpropoxy)quinazolin-4(3H)-one (319.36g / mol) in a dry single-necked flask, 60ml three Phosphorus oxychloride, then add DMF 0.5ml dropwise, and heat to reflux in an oil bath at 110°C for 1h.

[0037] 2: The unreacted phosphorus oxychloride was evaporated under reduced pressure to obtain a viscous liquid.

[0038] 3: Add 6.3g (0.025mol) of 3-chloro-4-fluoroaniline and 80ml of isopropanol directly to the obtained viscous liquid without purification, heat and reflux in a water bath at 90°C for 6h, then stop heating and cool down for crystallization.

[0039] 4: Wash the material with cold isopropanol after filtering, and obtain the crude product of gefitinib hydrochloride after drying.

[0040] 5: Dissolve the crude product in hot water and adjust the pH to 8-9 with saturated sodium bicarbonate solution, then filter to obtain the crude...

Embodiment 2

[0045] The preparation technology of Gefitinib of the present invention is as follows:

[0046] 1: Add 60ml SOCl to a dry one-necked flask 2 , 0.5ml of DMF, then add 10g of 7-methoxy-6-(3-morpholin-4-ylpropoxy)quinazolin-4(3H)-one (319.36g / mol), water bath 80°C Heat to reflux for 1h.

[0047] 2: Then evaporate the unreacted SOCl under reduced pressure 2 , to obtain a viscous liquid.

[0048] 3: Add 6.3g (0.025mol) of 3-chloro-4-fluoroaniline and 80ml of isopropanol directly to the obtained viscous liquid without purification, heat and reflux in a water bath at 90°C for 6h, then stop heating and cool down for crystallization.

[0049] 4: Wash the material with cold isopropanol after suction filtration, and obtain the crude product of gefitinib hydrochloride after drying.

[0050] 5: Dissolve the crude product in hot water and adjust the pH to 8-9 with saturated sodium bicarbonate solution, then filter to obtain the crude product of gefitinib.

[0051]6: Add crude gefitinib...

Embodiment 3

[0055] The preparation technology of Gefitinib of the present invention is as follows:

[0056] 1: Add 60ml SOCl to a dry one-necked flask 2 , 0.5ml of DMF, then add 10g of 7-methoxy-6-(3-morpholin-4-ylpropoxy)quinazolin-4(3H)-one (319.36g / mol), water bath 80°C Heat to reflux for 1h.

[0057] 2: Then evaporate the unreacted SOCl under reduced pressure 2 , to obtain a viscous liquid.

[0058] 3: Add 6.3g (0.025mol) of 3-chloro-4-fluoroaniline and 80ml of isopropanol directly to the obtained viscous liquid without purification, heat and reflux in a water bath at 90°C for 6h, then stop heating and cool down for crystallization.

[0059] 4: Wash the material with cold isopropanol after suction filtration, and obtain the crude product of gefitinib hydrochloride after drying.

[0060] 5: Dissolve the crude product in hot water and adjust the pH to 8-9 with saturated sodium bicarbonate solution, then filter to obtain the crude product of gefitinib.

[0061] 6: Add crude gefitini...

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Abstract

The invention relates to the preparation technology of high-purity gefitinib and belongs to the technical field of preparation of medical compounds. The technology is characterized in that 4-chlorine-7-methoxyl -6-(3-morpholin-4-ylpropoxy) quinazoline hydrochloride and 3-chlorine-4-fluoroaniline are in direct reaction, so as to obtain gefitinib hydrochloride, then gefitinib crude products can be obtained through neutralization, and finally, the high-purity gefitinib is obtained by post processing. In the invention, the the 4-chlorine-7-methoxyl-6-(3-morpholin-4-ylpropoxy) quinazoline hydrochloride and the 3-chlorine-4- fluoroaniline are in direct reaction, the production process is simplified, the production period is shortened, energy consumption is lowered, the types of all solvents are decreased at the same time, the use level of solution medium is reduced greatly, the production cost is obviously lowered, and pollutions caused by the solvents to human body and the environment are reduced; and in the invention, by preparing formylamine solvate, the purity of prepared gefitinib is high.

Description

technical field [0001] The invention relates to a preparation process of high-purity gefitinib, which belongs to the technical field of pharmaceutical compound preparation. Background technique [0002] The original preparation process of gefitinib is obtained by reacting 7-methoxy-6-(3-morpholin-4-ylpropoxy)quinazolin-4(3H)-one in excess acyl chloride reagent 4-Chloro-7-methoxy-6-(3-morpholin-4-ylpropoxy)quinazoline hydrochloride, then evaporate under reduced pressure to remove unreacted acid chloride reagent to obtain viscous liquid 4 -Chloro-7-methoxy-6-(3-morpholin-4-ylpropoxy)quinazoline hydrochloride, the viscous liquid is neutralized with lye to obtain 4-chloro-7-methoxy -6-(3-morpholin-4-ylpropoxyl) quinazoline, then extract with organic solvent and evaporate the organic solvent under reduced pressure to obtain 4-chloro-7-methoxyl group-6-(3- Morpholin-4-ylpropoxy)quinazoline solid. Then 4-chloro-7-methoxy-6-(3-morpholin-4-ylpropoxy) quinazoline reacts with 3-chlo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D239/94
Inventor 何茂群苗得足王福生刘元状赵永坤
Owner REYOUNG PHARMA
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