- Preparation method of lapatinib intermediate 2-(methanesulfonyl)ethylamine hydrochloride
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The invention discloses a preparation method of lapatinib intermediate 2-(methanesulfonyl)ethylamine hydrochloride. The preparation method comprises the steps of adopting 2-chloroethylamine hydrochloride (Compound 2) as a starting material, and under an alkaline condition, carrying out dimolecular substitution reaction on the starting material and sodium methyl mercaptide to prepare 2-methylmercapto ethylamine (Compound 3); then adopting water as a solvent, adding hydrochloric acid for salifying, and directly using hydrogen peroxide for oxidizing to obtain the 2-(methanesulfonyl)ethylamine hydrochloride (Compound 1). According to the preparation method provided by the invention, a synthetic route is short, the raw materials are simple and easy to get, the water is adopted as the solvent, the reaction condition is moderate, the after-treatment is simple, and the obtained product is good in quality and high in yield. The method can cause less three wastes, and is environmentally friendly and suitable for industrial production. The formula is shown in the specification.
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Paragraph 0011; 0029; 0032; 0033; 0035-0037
(2017/10/13)
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- Preparation method of Lapatinib side chain 2-(methyl sulfonyl) ethylamine salt
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The invention provides a preparation method of Lapatinib side chain 2-(methylsulfonyl) ethylamine salt. The method comprises the following steps: (A) performing reaction on one or two of 2-bromoethylamine and 2-bromoethylamine salt and di-tert-butyl dicarbonate methyl ester under the alkaline condition to obtain N-(Boc)-2-bromoethylamine; (B) performing reaction on the N-(Boc)-2-bromoethylamine and sodium methanesulfinate under the alkaline condition to obtain N-(Boc)-2- methylsulfonyl ethylamine; (C) acidifying the N-(Boc)-2-methylsulfonyl ethaneamine to obtain the Lapatinib side chain 2-(methylsulfonyl) ethylamine salt. The preparation method of the Lapatinib side chain 2-(methylsulfonyl) ethylamine salt, provided by the embodiment of the invention, avoids the occurrence of the problems that when an oxidization method is used for synthesizing a target product, unstable factors are many, and the operation of the obtained product is also unsafe. The preparation method has the advantages that the operation steps are simple and convenient; the molecule utilization degree is high; the reaction conditions can be easily controlled; the operation cost is low; the post treatment operation is simple and convenient; the purity of the obtained product is high.
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Paragraph 0054; 0059
(2017/08/28)
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- Lapatinib process for the preparation of intermediates
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The invention discloses a preparation method of a Tykerb intermediate. The preparation method of the Tykerb intermediate 1 comprises the following steps: (1) performing a nucleophilic substitute reaction on a compound as shown in a formula 3 and a compound as shown in a formula 4 under the effect of a catalyst in an organic solvent, wherein X is chlorine or bromine, M is sodium, potassium or zinc, and n is equal to 1 or 2; and (2) enabling a compound 2 obtained in the step (1) to react in a hydrogen chloride solution. According to the preparation method of the Tykerb intermediate 2, the nucleophilic substitute reaction is carried out on the compound as shown in the formula 3 and the compound as shown in the formula 4 under the effect of the catalyst in the organic solvent. The preparation method disclosed by the invention is simple to operate, the raw materials are cheap and easy to obtain, no environment pollution factor is caused, and the method is suitable for large-scale production in industry.
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Paragraph 0033; 0034
(2017/01/17)
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- 2 - (amino) ethyl methyl sulphone salt and wherein the intermediate preparation method
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The invention discloses a preparation method of a 2-(amino)ethyl methyl sulfone salt represented by formula 1. The preparation method comprises: (1) in an organic solvent and under the action of a substitution reaction catalyst, a compound 3 is reacted with a compound 4; and X is a halogen, and M is an alkali metal or an alkaline earth metal; and (2) a compound 2 prepared by the step (1) is reacted with an acidic aqueous solution to obtain a compound 1; n is equal to 1 or 2; m is equal to 1 or 2; and HmA is an organic acid or an inorganic acid. The invention also discloses a preparation method of the compound 2. The preparation method of the compound 2 comprises: 1) in an organic solvent and under the action of an alkali, a compound 5 is reacted with a halogenation reagent; and 2) in the organic solvent, under the action of the substitution reaction catalyst, the compound 4 is reacted with the compound 3 prepared by the step 1), X is a halogen, and M is an alkali metal or an alkaline earth metal. The preparation methods have low cost and easy availability of raw materials, have no environmental pollution factors, and are suitable for industrial mass production.
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Paragraph 0042; 0043
(2017/02/28)
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- THE NEW PREPARATION OF ALIPHATIC AMINES WITH SULPHONYL GROUP AND THEIR SALTS
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The present invention relates to a novel preparation method of sulfonyl alkylamine and salts thereof. The method of present invention comprises steps of: adopting sulfonates containing a sulfone moiety as starring material and ammonia oz amine as substituting agent which reacts with the starting material to prepare for the products. Furthermore, the present invention provides a new intermediate 2-(N,N- dibenzylamino) ethyl methyl sulfone and salts thereof obtained from the above novel preparation method and their use. In addition, the present invention also provides a novel salt of 2-(anuno) ethyl methyl sulfone prepared using 2-(amine) ethyl methyl sulfone hydrochloride and the use of novel salt. The present invention is not only advantageous for reducing environmental pollution, but also could be used for mass fabrication of 2-(amino) ethyl methyl sulfone and the salts thereof, in addition, the present invention is advantageous for preparing for the highly purified 2-(amine) ethyl methyl sulfone hydrochloride.
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Page/Page column 6
(2011/04/25)
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- 4-Aminoquinazoline derivatives and methods of use thereof
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This invention relates to novel 4-aminoquinazolines, their derivatives, pharmaceutically acceptable salts, solvates, and hydrates thereof. This invention also provides compositions comprising a compound of this invention and the use of such compositions in methods of treating diseases and conditions that are beneficially treated by administering inhibitors of the EGFR and HER-2.
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Page/Page column 15
(2008/06/13)
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- AZOLE COMPOUNDS
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The present invention provides a compound represented by the formula (I) wherein R1 is a hydrogen atom, a halogen atom, an optionally substituted hydrocarbon group, an optionally substituted heterocyclic group, an optionally substituted hydroxy group, an optionally substituted thiol group or an optionally substituted amino group, A is an optionally substituted cyclic amino group or -NR2-W-D wherein R2 is a hydrogen atom or an alkyl group, W is a bond or a divalent acyclic hydrocarbon group, and D is an optionally substituted cyclic group, an optionally substituted amino group or an optionally substituted acyl group, B is an optionally substituted hydrocarbon group or an optionally substituted heterocyclic group, X is an oxygen atom, a sulfur atom or an optionally substituted nitrogen atom, and Y is a bond or a divalent acyclic hydrocarbon group, or a salt thereof, which is useful for the prophylaxis or treatment of diabetic neuropathy and the like.
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- 3-cyanoquinolines, 3-cyano-1,6-naphthyridines, and 3-cyano-1,7-naphthyridines as protein kinase inhibitors
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This invention provides compounds of Formula (I), having the structure where T, Z, X, A, R1, R2a, R2b, R2c, R3, R4, and n are defined herein, or a pharmaceutically acceptable salt thereof which are useful as antineoplastic agents and in the treatment of osteoporosis and polycystic kidney disease.
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