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Synthetic method of epinastine hydrochloride impurity B
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A technology of epinastine hydrochloride and synthesis method, which is applied in the direction of measuring devices, instruments, bulk chemical production, etc.
Active Publication Date: 2017-09-01
HONGGUAN BIO PHARMA CO LTD
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Abstract
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At present, there is not a kind of synthetic method specifically for epinastine hydrochloride impurity B in the prior art
Method used
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Embodiment 1
[0027] Step 1: 6-aminomethyl-6,11-dihydro-5H-dibenzo[b,e]azepine preparation of
[0028]
[0029] Add methanol (200mL), 6-(phthalimidomethyl)-6,11-dihydro-5H-dibenzo-[b,e]azepine into a 500mL reaction flask (20g) and hydrazine hydrate (5.0g, 80% content). The temperature was raised to reflux for 4 hours, and the reaction was completed. Cool the reaction system to 5-10°C, filter, wash the filter cake with a small amount of methanol, spin the filtrate, add 100 mL of 5% sodiumhydroxide solution and 100 mL of dichloromethane, extract and separate the liquid, extract the aqueous phase with 50 mL of dichloromethane, and combine Organic phase, wash the organic phase with water 50mL×2, dry the organic phase with anhydroussodiumsulfate for 2 hours, filter and use the filtrate directly in the next reaction.
[0030] The second step: 3-amino-9,13-dihydro-1H-dibenzo[c,f]-imidazo[1,5-a]azepine preparation of
[0037] Step 1: 6-aminomethyl-6,11-dihydro-5H-dibenzo[b,e]azepine preparation of
[0038]
[0039] Add methanol (200mL), 6-(phthalimidomethyl)-6,11-dihydro-5H-dibenzo-[b,e]azepine into a 500mL reaction flask (20g) and hydrazine hydrate (3.3g, 80% content). The temperature was raised to reflux for 3 hours, and the reaction was completed. Cool the reaction system to 5-10°C, filter, wash the filter cake with a small amount of methanol, spin the filtrate to dry, add 100 mL of 5% sodiumhydroxide solution and 100 mL of dichloromethane, extract and separate the liquid, extract the aqueous phase with 50 mL of dichloromethane, and combine Organic phase, wash the organic phase with water 50mL×2, dry the organic phase with anhydroussodium sulfate for 2 hours, filter and use the filtrate directly in the next reaction.
[0040] The second step: 3-amino-9,13-dihydro-1H-dibenzo[c,f]-imidazo[1,5-a]azepine preparation of
[0047] Step 1: 6-aminomethyl-6,11-dihydro-5H-dibenzo[b,e]azepine preparation of
[0048]
[0049] Add methanol (200mL), 6-(phthalimidomethyl)-6,11-dihydro-5H-dibenzo-[b,e]azepine into a 500mL reaction flask (20g) and hydrazine hydrate (2.5g, 80% content). The temperature was raised to reflux for 5 hours, and the reaction was completed. Cool the reaction system to 5-10°C, filter, wash the filter cake with a small amount of methanol, spin the filtrate to dry, add 100 mL of 5% sodium hydroxide solution and 100 mL of dichloromethane, extract and separate the liquid, extract the aqueous phase with 50 mL of dichloromethane, and combine Organic phase, wash the organic phase with water 50mL×2, dry the organic phase with anhydroussodium sulfate for 2 hours, filter and use the filtrate directly in the next reaction.
[0050] The second step: 3-amino-9,13-dihydro-1H-dibenzo[c,f]-imidazo[1,5-a]azepine preparation of
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Abstract
The invention relates to the field of pharmaceutical technology and, and particularly relates to a preparation process of an epinastinehydrochlorideimpurity. The method comprises: firstly, using 6-(phthalimidomethyl)-6,11-dihydro-5H-dibenz[b,e]azepine (shown in the description) as a starting material, removing a protective group with hydrazine hydrate and then performing ring closure with cyanogenbromide to obtain 3- amino-9,13-dihydro-1H-dibenzo [c,f ]-imidazo [1,5-a] heterocyclic nitrogen (shown in the description) (epinastine), and finally reacting with a simple substance bromine to obtain the epinastinehydrochlorideimpurity B. The synthetic method of the epinastine hydrochlorideimpurity B has the advantages of being simple in process route, convenient to operate, good in selectivity and high in yield. The synthetic epinastine hydrochloride impurity B can be used as a control substance for testing a related substance of epinastine hydrochloride, can be applied in quality control of epinastine hydrochloride and related preparations thereof, and can be used for controlling the purity of the epinastine hydrochloride active pharmaceutical ingredients or preparations thereof.
Description
technical field [0001] The invention relates to the technical field of medicines, in particular to a preparation method of epinastine hydrochloride impurity. Background technique [0002] Allergic diseases are common clinical diseases. Allergic diseases have been threatening human health for a long time, especially in recent years, with the aggravation of environmental pollution, the incidence of such diseases has been increasing year by year. Epinastine hydrochloride is used to treat allergic diseases such as bronchial asthma, allergic dermatitis, urticaria, dermatitis, and common psoriasis, and has a very good curative effect. Epinastine hydrochloride chemical name: 3-amino-9,13-dihydro-1H-dibenzo[c,f]-imidazo[1,5-a]azepineHydrochloride, an oral antihistamine, has the following structural formula: [0003] [0004] EpinastineHydrochlorideStructural Formula [0005] Epinastine hydrochloride on H 1 Receptors are highly selective and affinity. At the same time, t...
Claims
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