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Synthesis method for epinastine hydrochloride

A technology for the synthesis of epinastine hydrochloride and its synthesis method, which is applied in the field of synthesis of epinastine hydrochloride, which can solve the problems of poor compound stability, threat to the safety of operators, and inability to guarantee cyanogen bromide, etc., so as to facilitate safe production , high safety, beneficial to the effect of environmental protection

Active Publication Date: 2015-12-16
ZHAOKE PHARMA GUANGZHOU
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0012] In this route, an azide compound will be used in the reaction for azidation reaction. The compound has poor stability and is extremely explosive. Due to its large amount of use in industrial production, it is extremely dangerous; secondly, the highly toxic substance bromine will be used in the reaction. Cyanide, which threatens the safety of operators, and cannot guarantee that cyanogen bromide will not remain in the prepared epinastine hydrochloride

Method used

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  • Synthesis method for epinastine hydrochloride
  • Synthesis method for epinastine hydrochloride
  • Synthesis method for epinastine hydrochloride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0061] Embodiment 1: the synthesis of compound shown in formula III

[0062] The reaction equation is as follows:

[0063]

[0064] In a 20L reactor, put 1Kg of the compound shown in formula II (6-aminomethyl-6,11-dihydro-5H-dibenzo[b,e]azepine maleate) and 6L of tert-butyl methyl ether , 8L of 30% aqueous sodium hydroxide solution, stirred at room temperature for 2 hours, after the completion of the reaction, the layers were left to stand, the organic phase was taken, dried over sodium sulfate, filtered and concentrated under reduced pressure to obtain 650g of the compound shown in formula III (mass yield 65% ).

Embodiment 2

[0065] Embodiment 2: the synthesis of compound shown in formula III

[0066] The reaction equation is as follows:

[0067]

[0068] In a 20L reactor, put 1Kg of the compound shown in formula II, 6L of dichloromethane, 8L of 30% aqueous sodium hydroxide solution, and stir at room temperature for 2 hours. After the reaction is complete, let the layers stand and take the organic phase, dry it with sodium sulfate, and filter Afterwards, it was concentrated under reduced pressure to obtain 570 g of the compound represented by formula III (mass yield 57%).

Embodiment 3

[0069] Embodiment 3: the synthesis (substitution reaction) of compound shown in formula V

[0070] The reaction equation is as follows:

[0071]

[0072] Dissolve 650 g of the compound represented by formula III in 1.5 L of acetone, slowly add dropwise an anhydrous acetone solution containing 575 g of the compound represented by formula IV, stir at 0°C for 3 hours, a large amount of light yellow solid precipitates, filter under reduced pressure, and filter the cake with acetone After washing and vacuum drying, 292 g of the compound represented by formula V was obtained (light yellow solid, mass yield 45%).

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Abstract

The invention discloses a synthesis method for epinastine hydrochloride. With a compound (6-aminomethyl-6,11-dihydro-5H-dibenzo [b, e] azepine maleate), shown in the formula II, being the initial raw material, epinastine hydrochloride is synthesized. By the utilization of the synthesis method for epinastine hydrochloride, epinsastine hydrochloride can be effectively synthesized, and the method has the advantages of being high in synthesis efficiency, safe in production, simple in technology operation, short in production period and the like and is more suitable for large-scale and industrialized production of epinastine hydrochloride.

Description

technical field [0001] The invention relates to the technical field of medicine, in particular to a synthesis method of epinastine hydrochloride. Background technique [0002] The English name of Epinastine Hydrochloride is epinastinehydrochloride, the chemical name is 3-amino-9,13-dihydro-1H-dibenzo[c,f]-imidazo[1,5-a]azepine hydrochloride, Its structural formula is as follows: [0003] [0004] Epinastine hydrochloride is used for the treatment of bronchial asthma, allergic dermatitis, urticaria, eczema, dermatitis and common psoriasis (psoriasis), has a strong inhibitory effect on bronchoconstriction caused by histamine and bradykinin, and It has no inhibitory effect on bronchoconstriction caused by other chemical mediators, and is one of the most effective non-sedative histamine H1 receptor antagonists acting on peripheral nerves. There was no significant difference in pharmacological activity between D-epistine, L-epistine and racemic epinastine. Epinastine hydroc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D487/04A61P11/06A61P37/08A61P17/00A61P17/06
CPCC07D487/04
Inventor 李小羿左从菊戴向荣夏良迟权德任建
Owner ZHAOKE PHARMA GUANGZHOU