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Purification method of N-(2,2-diethoxyethyl)phthalimide

A technology for phthalimide and crude phthalimide, which is applied in the field of medicine and chemical industry, can solve problems such as the influence of intermediate quality and adverse synthesis quality of Recapab, and achieve low-cost separation and guarantee Synthetic quality effects

Inactive Publication Date: 2019-02-22
CHONGQING BEISHENG PHARMA TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] N-(2,2-diethoxyethyl)phthalimide is prepared by condensation of potassium phthalimide and bromoethanol diethyl acetal. The intermediate of the fragment, the existing technology does not purify the intermediate, resulting in a slight impact on the quality of the subsequent intermediate, which is not conducive to the synthetic quality of recaprabab

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] The purification of N-(2,2-diethoxyethyl)phthalimide has the following steps,

[0024] 1) Dissolve 100 g of crude N-(2,2-diethoxyethyl) phthalimide (purity: 92.4%) purchased from Chongqing Kanghe Yuecheng Pharmaceutical Technology Co., Ltd. in 250 g of dichloromethane , control the temperature of the system at 0-40° C. and stir for 1 hour to obtain a crude product solution;

[0025] 2) Press-filter the crude product solution to obtain a filtrate, control the temperature at 45-65° C., concentrate under reduced pressure until no liquid flows out, and a white solid is precipitated to obtain a wet product;

[0026] 3) Cool the wet product to 0-30°C, add 420g of ethanol to dissolve, stir, raise the temperature to 30-50°C and stir for 3 hours, after the system is dissolved and clarified, the refined solution is obtained;

[0027] 4) Cool the fine solution to 0-30°C, add 300g of drinking water dropwise to the solution, control the dropping process at 0-30°C, stir for 2 hours ...

Embodiment 2

[0031] 1) Dissolve 100 g of crude N-(2,2-diethoxyethyl) phthalimide (purity: 92.4%) in 250 g of dichloromethane, control the system temperature at 0-40°C and stir for 1 hour , to obtain the crude product solution;

[0032] 2) Press-filter the crude product solution to obtain a filtrate, control the temperature at 45-65° C., concentrate under reduced pressure until no liquid flows out, and a white solid is precipitated to obtain a wet product;

[0033] 3) Cool the wet product to 0-30°C, add 420g of ethanol to dissolve, stir, raise the temperature to 30-50°C and stir for 3 hours, after the system is dissolved and clarified, the refined solution is obtained;

[0034] 4) Cool the fine solution to 0-30°C, add 300g of drinking water dropwise to the solution, control the dropping process at 0-30°C, stir for 2 hours after dropping, and filter with suction to obtain 108.5g of filter cake;

[0035] 5) The obtained filter cake was blast-dried at a temperature of 45-65° C., and dried to ...

Embodiment 3

[0038] 1) Dissolve 100 g of crude N-(2,2-diethoxyethyl) phthalimide (purity: 92.4%) in 250 g of dichloromethane, control the system temperature at 0-40°C and stir for 1 hour , to obtain the crude product solution;

[0039] 2) Press-filter the crude product solution to obtain a filtrate, control the temperature at 45-65° C., concentrate under reduced pressure until no liquid flows out, and a white solid is precipitated to obtain a wet product;

[0040] 3) Cool the wet product to 0-30°C, add 420g of ethanol to dissolve, stir, raise the temperature to 30-50°C and stir for 3 hours, after the system is dissolved and clarified, the refined solution is obtained;

[0041] 4) Cool the fine solution to 0-30°C, add 300g of drinking water dropwise to the solution, control the dropping process at 0-30°C, stir for 2 hours after dropping, and filter with suction to obtain 108.5g of filter cake;

[0042] 5) The obtained filter cake was blast-dried at a temperature of 45-65° C., and dried to ...

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Abstract

A purification method of N-(2,2-diethoxyethyl)phthalimide comprises the following steps: 1) dissolving crude N-(2,2-diethoxyethyl)phthalimide in an alkane organic solvent and / or a ketone organic solvent, and controlling system temperature at 0-40 DEG C until complete dissolution to obtain a crude product solution; 2) filtering the crude product solution obtained in step 1), taking a filtrate, andconcentrating the filtrate under reduced pressure until the solvent is dried by evaporation to obtain a wet product; 3) dissolving the wet product obtained in step 2) in an alkane organic solvent and / or a ketone organic solvent and / or an alcohol organic solvent until complete dissolution to obtain a refined product solution; 4) cooling the refined product solution obtained in step 3) to 0-30 DEG C, adding water dropwise, performing stirring and filtering after addition, taking a filter cake, and drying the filter cake to obtain pure N-(2,2-diethoxyethyl)phthalimide. The purification process issimple and mild, purity of N-(2,2-diethoxyethyl)phthalimide can be improved effectively to 99% or higher, and synthesis quality of rucaparib is guaranteed.

Description

technical field [0001] The invention relates to the field of medicine and chemical industry, in particular to a method for purifying N-(2,2-diethoxyethyl)phthalimide. Background technique [0002] N-(2,2-diethoxyethyl)phthalimide is prepared by condensation of potassium phthalimide and bromoethanol diethyl acetal. For the intermediate of the fragment, the prior art has not purified the intermediate, resulting in a slight impact on the quality of the subsequent intermediate, which is not conducive to the synthetic quality of recaprabib. Contents of the invention [0003] The purpose of this invention is to provide a kind of purification method of N-(2,2-diethoxyethyl) phthalimide for the deficiencies in the prior art. The purification process is simple and mild, and can effectively improve the N The purity of -(2,2-diethoxyethyl)phthalimide is over 99%, which ensures the synthetic quality of recaprabib. [0004] Technical scheme of the present invention is: a kind of puri...

Claims

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Application Information

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IPC IPC(8): C07D209/48
CPCC07D209/48
Inventor 潘敬坤尹彪
Owner CHONGQING BEISHENG PHARMA TECH CO LTD
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