2-(4-chlorophenylacetyl)benzoic acid synthesis process
A synthesis technique and chlorophenylacetyl technology are applied in the preparation of carboxylic acid anhydride, organic chemistry, etc., can solve problems such as low synthesis yield, and achieve the effect of improving yield
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Embodiment 1
[0011] Example 1: Add p-chlorophenylacetic acid, phthalic anhydride and newly melted sodium acetate in proportion to the reaction kettle, heat rapidly to about 240°C, stir and react at 240-250°C for 3 hours, and the reaction process The water produced in the process is exported from the tail joint; then put the reaction mixture into an open heat-resistant container while it is hot, cool it while stirring, add cold absolute ethanol, heat to dissolve the solid as much as possible, filter after cooling, and use anhydrous Washed with ethanol, filtered and dried.
[0012] Add the obtained solid into the solution formed by sodium hydroxide and water, heat, stir and reflux for 3 hours, cool, add water to dilute, acidify to PH 2-3 with 20% hydrochloric acid, stir, cool, and a solid oily substance precipitates out , filtered, and dried to obtain a crude product. The crude product was dissolved in acetone, the insoluble matter was filtered off, the acetone was evaporated, and the residu...
Embodiment 2
[0013] Example 2: Add p-chlorophenylacetic acid, phthalic anhydride and newly melted sodium acetate in proportion to the reaction kettle, heat rapidly to about 250°C, stir and react at 240-250°C for 3 hours, and the reaction process The water produced in the process is exported from the tail joint; then put the reaction mixture into an open heat-resistant container while it is hot, cool it while stirring, add cold absolute ethanol, heat to dissolve the solid as much as possible, filter after cooling, and use anhydrous Washed with ethanol, filtered and dried.
[0014] Add the obtained solid into the solution formed by sodium hydroxide and water, heat, stir and reflux for 4 hours, cool, add water to dilute, acidify to PH 2-3 with 20% hydrochloric acid, stir, cool, and a solid oily substance precipitates out , filtered, and dried to obtain a crude product. The crude product was dissolved in acetone, the insoluble matter was filtered off, the acetone was evaporated, and the residu...
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