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Method for preparing Erlotinib hydrochloride crystal form A
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A technology for erlotinib hydrochloride and crystal form, which is applied in the field of preparation of erlotinib hydrochloride crystal form A, can solve the problems of inability to stably obtain the product of crystal form A, uncontrollable process conditions, and inability to quantify parameters, etc. To achieve the effect of feasible and controllable operation, high reproducibility and low cost
Inactive Publication Date: 2011-07-20
ZHEJIANG JIUZHOU PHARM CO LTD
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[0018] The present invention improves the process on the basis of the prior art (US5747498) described in the background art, and solves the technical problems of uncontrollable process conditions and unquantifiable parameters in the prior art, which lead to the inability to stably produce crystal A Type product, it is easy to produce the problem of crystal form B in the process of preparing erlotinib hydrochloride crystal form A, and a preparation method of erlotinib hydrochloride crystal form A is proposed, which can produce pure A crystal product
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Embodiment 1
[0043] Embodiment 1 (preparation of erlotinib hydrochloride crystal form A)
[0044] In a clean and dry 250mL four-necked flask, put 10g of erlotinib free base monomer, 100mL of dichloromethane and 20mL of methyl tert-butyl ether, start stirring, cool to -20~-15℃ in ice water, start slowly The concentration of hydrogen chloride added dropwise is 2.0mol.L -1 14.0mL of methyl tert-butyl ether hydrogen chloride solution, drop it in 0-1 hour, after the dropwise addition, keep warm for 0.1-1 hour, after heat preservation, filter, rinse the wet product with 10mL methyl tert-butyl ether, pump After drying, put it in a vacuum oven at 20-30°C for drying to obtain a dry product: 10.9 g, yield: 100%.
Embodiment 2
[0045] Embodiment 2 (preparation of erlotinib hydrochloride crystal form A)
[0046] In a clean and dry 250mL four-neck flask, put 10g of erlotinib free base monomer and 100mL of acetone, start stirring, cool to -20~-15°C with ice water, and slowly add hydrogen chloride with a concentration of 2.0mol.L -1 14.0mL of methyl tert-butyl ether hydrogen chloride solution, drop it in 0-1 hour, after the dropwise addition, keep warm for 0.1-1 hour, after heat preservation, filter, rinse the wet product with 10mL methyl tert-butyl ether, pump After drying, put it in a vacuum oven at 20-30°C for drying to obtain a dry product: 10.9 g, yield: 100%.
Embodiment 3
[0047] Embodiment 3 (preparation of erlotinib hydrochloride crystal form A)
[0048] In a clean and dry 500mL four-neck flask, put 10g of erlotinib free base monomer and 18.5mL of toluene to start stirring, cool to -5~0°C with ice water, and slowly add hydrogen chloride with a concentration of 0.1mol.L -1 254mL of anisole hydrogen chloride solution, drop it in 1.5-2.5 hours, drop it, keep it warm for 1.5-2.5 hours, keep it warm, filter, rinse the wet product with 10ml anisole, drain it, put it in Dry in a vacuum oven at 30°C to obtain a dry product: 10.7 g, yield: 99.1%.
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Abstract
The invention belongs to the technical field of chemical pharmacy, and in particular relates to a method for preparing an Erlotinib hydrochloride crystal form A. The method solves the technical problems that the prior art has uncontrollable process conditions, un-quantitative parameters and the like to cause the problems that products of the crystal form A cannot be prepared stably and a crystal form B is easy to generate in the process of preparing the Erlotinib hydrochloride crystal form A. The method comprises the following steps: mixing an Erlotinib free alkali monomer with an organic solvent, then dropping ether chlorine hydride solution, and preparing the Erlotinib hydrochloride crystal form A at a low temperature. The method has the advantages of high process stability, practicableand controllable operation, low cost and high reproducibility, can obtain a pure product of the crystal form A with high yield, is more suitable for the industrial production of preparing the Erlotinib hydrochloride crystal form A, and has high economic benefit.
Description
technical field [0001] The invention relates to the technical field of chemical industry and pharmacy, and more specifically, relates to a preparation method of erlotinib hydrochloride crystal form A. Background technique [0002] The phenomenon that the same element or compound forms crystals with completely different structures, shapes, and physical properties under different conditions is called polymorphism. Polymorphism exists widely in organic medicines. The crystallization of polymorphic medicines mostly belongs to molecular lattice, and different crystal forms are produced with different process conditions. Due to the difference in crystal type and purity of the same drug, there may be significant differences in the physical properties (such as solubility, dissolution rate, melting point, etc.) and stability (crystal form and chemical stability) of the drug, thus affecting the safety and effectiveness of the drug. Sex can make a difference. [0003] For APIs with p...
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Application Information
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