Industrial preparation method for 3-amino phenylacetic acid
A technology of aminophenylacetic acid and p-nitrophenylacetonitrile, which is applied in the field of preparation of 3-aminophenylacetic acid, can solve the problems of nitration products being very complex and difficult to separate, and achieves the effects of high selectivity and mild reaction conditions
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[0028] Add 200ml of water into the three-necked flask, add 80g of iron powder under mechanical stirring, reflux with 4ml of acetic acid for 30min, cool down to 90-95°C, add 64.8g of p-nitrophenylacetonitrile in batches, reflux for 4hr after the addition, and cool down to 80°C , add 200ml of dichloroethane, filter with suction, wash the filter cake with hot dichloroethane, separate the organic layer, and precipitate under reduced pressure to obtain 50.1 g of the product p-aminophenylacetonitrile, with a yield of 95%.
[0029] Add 24.5ml acetic acid to 52.8g p-aminophenylacetonitrile, add dropwise 24.5ml acetic anhydride at room temperature, continue to react for 1hr after dripping, the reaction solution is poured into ice water, and suction filtration obtains 63.3g of product p-acetamidophenylacetonitrile, the yield 91%.
[0030] Add 91ml of 60% nitric acid dropwise to 91ml of concentrated sulfuric acid, add 34.8g of p-acetaminophenylacetonitrile in batches under ice water cool...
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