- holds the non-rope to divide method for the preparation of intermediates
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The invention relates to a preparation method of a tofisopam intermediate 3-[2-(3,4-dimethoxy benzoic acyl)-4,5-dimethoxyphenyl]-penta-2-ketone, and belongs to the technical field of pharmaceutical synthesis. The method comprises the following step: carrying out reaction on 1-(3,4-dimethoxy-phenyl)-3-ethyl-5,6-dimethoxy-2-methyl-indan as an initial material, copper compounds as catalysts, and hydrogen peroxide as an oxidant under an acid condition, so as to prepare the tofisopam intermediate 3-[2-(3,4-dimethoxy benzoic acyl)-4,5-dimethoxyphenyl]-penta-2-ketone. According to the preparation method, the content of heavy metals in the wastewater is greatly lowered, chromium compounds with carcinogenesis are avoided, the production capacity of tofisopam is released, and the environment is protected.
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Paragraph 0034-0035
(2017/02/24)
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- One-pot synthesis of 2,3-benzodiazepines from arynes and β-diketones
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Novel one-pot synthesis of 2,3-benzodiazepines from aryne precursors was accomplished. Tofisopam, well-known anxiolytics, could be synthesized via C-C bond insertion of 4,5-dimethoxybenzyne with 2-ethyl-1-(3,4-dimethoxyphenyl)- butane-1,3-dione, followed by the reaction with hydrazine hydrate in a one-pot operation. This protocol is applicable to the synthesis of other biologically active 2,3-benzodiazepines, such as Girisopam and Nerisopam.
- Okuma, Kentaro,Tanabe, Yukiko,Itoyama, Ryoichi,Nagahora, Noriyoshi,Shioji, Kosei
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supporting information
p. 1260 - 1262
(2013/10/22)
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- PROCESS FOR THE PREPARATION OF 3-[2-(3,4-DIMETHOXYBENZOYL)-4,5- DIMETHOXYPHENYL] -PENTAN-2-ONE
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The invention relates to a new process for the preparation of 3-[2-(3,4-dimethoxybenzoyl)-4,5- dimethoxyphenyl]-pentan-2-one of the formula (I), starting from a compound of the general formula (II) and subjecting the thus-obtained compound of the general formula (IV) to hydrolysis. The compound of the formula (I) is a pharmaceutical intermediate, which can be used for the preparation of an anxiolytic, namely tofisopam (INN).
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- PROCESS FOR THE PREPARATION OF 3-[2-(3,4-DIMETHOXY-BENZOYL)-4,5-DIMETHOXY-PHENYL]-PENTAN-2-ONE
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The invention relates to a process for the preparation of 3-[2-(3,4-dimethoxy-benzoyl)-4,5-dimethoxy-phenyl]-pentan-2-one of the Formula (I) starting from a compound of the general Formula (II) (wherein R1 and R2 each stands for C1-4-alkyl or together form C2-6-alkylene).
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