- Preparation method of butylphthalide
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The invention discloses a of butylphthalide. The preparation method comprises the following steps: with phthalic anhydride as a starting material, carrying out condensation, hydrolysis, reduction andesterification reactions to obtain butylphthalide. According to the preparation method, reaction raw materials are easy to obtain, operation is simple, reaction conditions are relatively mild, requirements on equipment is low, crude drugs with a purity of more than 99.80% and meeting medicinal requirements can be obtained without rectification, and the preparation method is suitable for industrialproduction.
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Paragraph 0063-0064; 0071-0072
(2020/11/26)
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- Synthetic method of food additive tetrabutylphthalide and application thereof in seasoning (by machine translation)
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The synthesized product is used as a main effective component of medicinal plant volatile oil such as angelica sinensis, wallichii and the like; therefore, the product can replace a large amount of natural plants or natural plant extracts, so that the cost is greatly reduced by using the Grignard reagent of natural plants or natural plant extracts of the intermediate 3 - 3 - hydroxyl -3 -butyl -1 (3H) and the traditional Grignard reagent. (by machine translation)
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Paragraph 0036; 0039
(2020/06/09)
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- A controllable bulk drug product and its preparation method
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The present invention provides a butyl phthalide raw material drug product with the butyl phthalide content not less than 99.0%; the raw material drug is stable in quality, and can ensure the clinical curative effect and drug safety of a butyl phthalide preparation.
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Paragraph 0081-0083
(2018/12/13)
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- Butyphthalide preparation method
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The invention provides a butyphthalide preparation method which comprises the following steps: S1) utilizing raney nickel as a catalyst, performing hydrogenation reaction on butylidene phthalide in an alcohol solvent and reducing pressure to remove the solvent to obtain a first intermediate; S2) mixing the first intermediate, sodium hydroxide and water to react, then utilizing dichloromethane to wash a reaction system, then adding the alcohol solvent and performing acid adjusting reaction to obtain a second intermediate; S3) performing cyclization reaction on the second intermediate in an acid organic solvent to obtain butyphthalide. Compared with the prior art, the butyphthalide preparation method disclosed by the invention utilizes the alcohol solvent and the dichloromethane as reaction or extraction solvents; the alcohol solvent and the dichloromethane both can be effectively recycled and is low in cost, so that production cost is greatly reduced; through hydrolyzing purification and acid adjusting filtration purification, high-purity butyphthalide meeting a preparation requirement can be obtained in higher yield; the steps of reducing pressure and rectifying are avoided, and operation is simple.
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Paragraph 0057; 0058; 0059; 0066; 0067; 0068
(2017/10/13)
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- Method used for preparing n-butylphathlide via one pot method
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The invention belongs to the technical field of chemical synthesis, and more specifically relates to a method used for preparing n-butylphathlide via one pot method. The method comprises following steps: phthalic anhydride and valeric anhydride are subjected to a first step reaction under catalytic action of anhydrous sodium acetate, and generated n-pentanoic acid is collected via reduced pressure distillation; a sodium hydroxide solution of sodium borohydride is added into a reaction liquid for a second step of reaction; dichloromethane is used for extracting impurities; pH value is adjusted to be smaller than 7 with an acid for a third step of reaction, dichloromethane is used for extracting, and n-butylphathlide is obtained via concentration. The method is high in yield, low in cost, is safe, and is friendly to the environment.
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Paragraph 0023
(2017/01/19)
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- High-content butylphenyl phthaleine composition and preparation method thereof
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The invention provides a high-content butylphenyl phthaleine composition. The butylphenyl phthaleine pharmaceutical composition comprises the following components: active component butylphenyl phthaleine, wherein the butylphenyl phthaleine content is no less than 99.5%; impurity with amount of no greater than 0.5% by metering weight percentage sum of butylphenyl phthaleine, wherein after placing for 24 months under normal condition, the butylphenyl phthaleine content is no less than 99.0%; and the impurity with amount of no greater than 1.0% by metering the weight percentage sum of butylphenyl phthaleine.
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Paragraph 0052
(2017/06/07)
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- Catalytic enantioselective synthesis of chiral phthalides by efficient reductive cyclization of 2-acylarylcarboxylates under aqueous transfer hydrogenation conditions
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A new diamine ligand for asymmetric transfer hydrogenation (ATH) was discovered. The reductive cyclization of 2-acylarylcarboxylates was found to proceed highly stereoselective by the new Ru complex-catalyzed ATH and subsequent In situ lactonization under aqueous conditions. It enables efficient access to a wide variety of 3-substituted phthalides In enantiomerically pure form.
- Zhang, Bo,Xu, Ming-Hua,Lin, Guo-Qiang
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supporting information; experimental part
p. 4712 - 4715
(2009/12/08)
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- Incorporation of molecular nitrogen into organic compounds IV. Novel lactam synthesis by nitrogenation of enol lactones
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Enol lactones 7, which are readily prepared from o-haloacetophenone derivatives 15 by palladium-catalyzed carbonylation, react with the titanium-isocyanate complex (1) generated by fixation of CO2 with titanium-nitrogen complex to give the isoindolinone derivatives 8 in good yields.
- Uozumi, Yasuhiro,Mori, Eiko,Mori, Miwako,Shibasaki, Masakatsu
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- Novel Lactam Synthesis by Use of a Combination System of Carbonylation and Nitrogenation
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An amide unit was constructed from aryl halide and titanium-isocyanate complex prepared from TiCl4 under atmospheric pressure of molecular nitrogen and carbon monoxide in the presence of a palladium catalyst.With this combination system of carbonylation and nitrogenation, isoindolinone and quinazolinone derivatives were synthesized from o-halophenyl alkyl ketone in one step.The reaction proceeds through the oxidative addition of enol lactone, generated by palladium-catalyzed carbonylation to o-halophenyl alkyl ketone, to titanium-isocyanate complex.
- Uozumi, Yasuhiro,Kawasaki, Naofumi,Mori, Eiko,Mori, Miwako,Shibasaki, Masakatsu
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p. 3725 - 3727
(2007/10/02)
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