- Method for preparing blonanserin intermediate (BN-04)
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The invention discloses a preparation method of a key Bnanserin intermediate (BN-04). The method comprises the following steps: reacting 4-(4-fluorophenyl)-5,6,7,8,9,10-hexahydrocyclooctanopyridine-2(1H)-ketone (BN-03) with a chlorinating reagent hydrochloric acid in acetic anhydride at a low temperature, and after the reaction, recovering a solvent under reduced pressure; cooling to below 50 DEGC, adding dichloromethane and water, adjusting the pH value with ammonia water, layering, drying with anhydrous sodium sulfate, and recovering the dichloromethane to be clean under reduced pressure; adding a proper amount of ethanol to be completely dissolved, cooling, crystallizing and filtering to obtain 2-chloro-4-(4-fluorophenyl)-5,6,7,8,9,10-hexahydrocyclooctanopyridine (BN-04). Compared withthe prior art, cheap and high-quality hydrogen chloride is taken as a chlorinating reagent, a high-temperature (170 DEG C) reaction is avoided, the generation of impurities is reduced, repeated recrystallization in the refining process is avoided, and acetic anhydride can be repeatedly used as a reaction solvent. Green, safe and environment-friendly modern production can be realized.
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Paragraph 0025-0035
(2019/12/25)
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- METHOD OF PRODUCING BLONANSERIN
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PROBLEM TO BE SOLVED: To provide a method of producing blonanserin. SOLUTION: The invention relates to an improved method of producing high-purity 2-(4-ethyl-1-piperazinyl)-4-(4-fluorophenyl)-5,6,7,8,9,10-hexahydrocycloocta[b]pyridine (INN name blonanserin). The method is implemented through four successive steps starting from C1-4-alkyl 4-fluorobenzoate. The invention also relates to a method of producing 3-(4-fluorophenyl)-3-oxopropanenitrile (BLON1) being an intermediate. SELECTED DRAWING: None COPYRIGHT: (C)2018,JPOandINPIT
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- Blonanserin and preparation method thereof
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The invention relates to Blonanserin and a preparation method thereof. The preparation method comprises the following specific steps that firstly, the compound shown in the formula III is reacted with a chlorinating agent, namely phosphenylic oxychloride, and the compound shown in the formula II is obtained; secondly, in the presence of potassium iodide, the compound shown in the formula II is reacted with N-ethylpiperazine, and the compound shown in the formula I, namely Blonanserin, is obtained. The preparation method has the advantages shown in the description.
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Paragraph 0087; 0088; 0093; 0098; 0103; 0108
(2017/07/21)
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- In the preparation method of the midbody blonanserin (by machine translation)
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The present invention provides a process for the preparation of intermediates blonanserin key, comprises the following steps: the 4 [...] (the 4 [...] phenyl) - 3 the [...] 5, 6, 7, 8, 9, 10-hexahydro cyclooctane and pyridine -2 (1H)-one and chloropivaloyl reagent in the reaction under a certain condition, after the reaction, the reactants are poured into ice water, pH value is adjusted with ammonia water, stirring, filtering or offcenter the 2 [...] -4 the [...] (the 4 [...] phenyl) - 5, 6, 7, 8, 9, 10-hexahydro cyclooctane [b] pyridine (compound I) crude; compound I hot ethanol is dissolved, decolourizations, recrystallization, the refined product obtained. Compared with the prior art, the method, in the process of refining a plurality of extraction, the solvent loss in the process, the operation is simple and easy to operate, has improved the purity of the product and yield, amplifying and industrial production processes. (by machine translation)
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Paragraph 0026; 0027; 0028; 0029
(2016/11/02)
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- Method for Preparing Blonancerin with Mild Condition
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The present invention provides a novel producing method of blonanserin. A producing method of the present invention has mild reaction temperature and short reaction time, can produce high-purity and high-yield blonanserin and is suitable for mass producti
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Paragraph 0046; 0047; 0048
(2016/10/10)
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- An investigation into formation of impurities during synthesis of blonanserin
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During the process development of Blonanserin (1 ), we have observed formations of unknown impurities are in the final product at enhanced levels which was identified as Des ethyl impurity, di-N-ethylpiperazine impurity, Chloro impurity and des-fluoro impurity. The present work involves detailed optimization studies directed toward the development of an efficient process for the commercial production of Blonanserin substantially free from the chloro impurity and other impurities.
- Sudarshan Rao,Nageswara Rao,Uma Sankara Sastry,Muralikrishna,Jayashree
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p. 5928 - 5930
(2015/02/19)
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- Syntheses and properties of the major hydroxy metabolites in humans of blonanserin AD-5423, a novel antipsychotic agent
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Two major metabolites in humans of blonanserin, 2-(4-ethyl-1-piperazinyl)- 4-(4-fluorophenyl)-5,6,7,8,9,10-hexahydrocycloocta-[b]pyridine (code name AD-5423), were synthesized. The first, 7-hydroxylated AD-5423, was synthesized through a four-step process
- Ochi, Takeshi,Sakamoto, Masato,Minamida, Akira,Suzuki, Kenji,Ueda, Tomohiko,Une, Teruaki,Toda, Hiroshi,Matsumoto, Kazuya,Terauchi, Yoshiaki
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p. 1055 - 1059
(2007/10/03)
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