Indeno oxa-carboxylic acid derivative with bioactivities and method for preparing same
A technology of indenooxacarboxylic acid and biological activity, applied in the field of indenooxacarboxylic acid derivatives and their preparation
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Embodiment 1
[0045] This example illustrates the preparation of compound 01 in Table 1.
[0046]
[0047] Add chlorobenzene (VII-01646.0g) and aluminum trichloride (193g) in a reaction flask (1000mL) equipped with a stirrer, thermometer and tail gas receiver, and add 3-chloropropionyl chloride ( 170g), after dripping, keep warm at 50-60°C until the reaction is complete, slowly add the reactant to a solution composed of concentrated hydrochloric acid (80.0g) and crushed ice (2000g), and suction filter the precipitated solid crude product. Alcohol solvents such as ethanol Recrystallization gave (VI-01) 276.6g, content 99.0% (GC).
[0048] Slowly add (VI-01)(12.6)g n-octane (200mL) solution dropwise to the mixed solution of concentrated sulfuric acid (100mL) and n-octane (50mL) at 90-110°C, after the drop is complete, cool to room temperature, The n-octane layer was decanted, and the reaction solution was slowly poured onto crushed ice (1000 g) while stirring, and the precipitated solid w...
Embodiment 2
[0054] This example illustrates the preparation of compound 12 in Table 1.
[0055]
[0056] Add benzene (VII-12448.0g) and aluminum trichloride (192.9g) to a 1000mL reaction flask equipped with a stirrer, thermometer and tail gas receiver, and add 3-chloropropionyl chloride (168g) dropwise at 10-25°C After dropping, keep warm at 50-60°C until the reaction is complete. Slowly add the reactant to a solution consisting of 80.0 g of concentrated hydrochloric acid and 2000 g of ice water, cool and filter with suction to obtain the crude product, and recrystallize from an alcohol solvent such as ethanol to obtain (VI- 12) 228.4g, content 97.2%.
[0057] Slowly add (VI-12) (10.1g) n-octane (200mL) solution dropwise to the mixed solution of concentrated sulfuric acid (100mL) and n-octane (50mL) at 90-110°C, after the dropwise completion, cool to room temperature, The n-octane layer was decanted, and the reaction solution was slowly poured onto crushed ice (1000 g) while stirring,...
Embodiment 3
[0064] Preparation of suspending agent: Dilute 2-6% wetting and dispersing agent in 4-10% antifreeze, and slowly add a certain amount of water to the solution, then add in sequence under high-speed shearing knife stirring 5-80% active compound of formula (I) provided by the present invention, 0.01-0.05% preservative, 0.01-0.05% defoamer and thickener, etc. Finally, it is poured into a sand mill for grinding, and then the solvent is added to volume. It can be diluted with water to any desired concentration when used.
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Abstract
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