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CAS No. : | 2827-56-7 | MDL No. : | MFCD02093080 |
Formula : | C3H6ClN3O2 | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | WEOHANUVLKERQI-UHFFFAOYSA-N |
M.W : | 151.55 | Pubchem ID : | 12472963 |
Synonyms : |
|
Chemical Name : | 1-Aminohydantoin hydrochloride |
Signal Word: | Warning | Class: | N/A |
Precautionary Statements: | P305+P351+P338 | UN#: | N/A |
Hazard Statements: | H315-H319 | Packing Group: | N/A |
GHS Pictogram: |
* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Ca. 70% | Add 90kg of aminohydantoin hydrochloride, 590kg of water and 66L of acetic acid in a 1000L reaction pot.Mechanical stirring was started, and ice water was cooled to a temperature below 20 C, and 106 L of concentrated sulfuric acid was slowly added thereto, and the dropwise addition was completed in about 1.5 hours.After stirring for 30 to 60 minutes, 160 kg of 5-Nitro-2-furaldehyde diacetate was gradually added, and finally 97 wt% of ethanol 118 L was added.The steam was heated to an internal temperature of 90 C.The reaction was kept warm and stirred for 3 hours, and the reaction solution became cloudy. Two gradients are cooled down to an internal temperature of 5 to 10 CSpecifically, in the present embodiment, first, the purified water is cooled to an internal temperature of 50 C, and then cooled to an internal temperature of 5 to 10 C with ice water.Gradually more yellow solids precipitated.The mash was filtered, and the filter cake was washed with a large amount of purified water in a near neutral state (pH = 6 to 7), and then washed with 95% by weight of ethanol.The crude product was placed in an oven and dried at 70 to 80 C for 3 hours.A yellow crystalline powder, i.e., 1-[[(5-nitro-2-furyl)methylene]amino]-2,4-imidazolidinedione, was obtained. Specifically, in the present embodiment, 1-[[(5-nitro-2-furyl)methylene]amino]-2,4-imidazolidinedione and N,N-dimethylformamide,The charge ratio of purified water and 95% by weight of ethanol is: 1-[[(5-nitro-2-furyl)methylene]amino]-2,4-imidazolidinedione (kg):N,N-dimethylformamide (L): purified water (L): 95% by weight of ethanol (L) = 1: 1.1: 2.2: 1.1.The above feed ratio of N,N-dimethylformamide was added to a 500 L reaction vessel, and 1-[[(5-nitro-2-furanyl)methylene]amino]-2,4-imidazolidine was added. The diketone was stirred at room temperature (23 C) for 40 minutes.Open compressed air for pressure filtration. The material was hydraulically poured into a crystallizing pot, stirred, and purified water was added dropwise to precipitate a yellow solid.Stirring was maintained for 30 minutes.The mash is filtered to obtain a filter cake.The filter cake was washed with a large amount of purified water, and then washed with three times or four times with 95 wt% of ethanol, and dried to obtain a cake.The filter cake was placed in an oven and dried at 70 to 80 C for 3 hours to obtain a yellow crystalline powder, that is, the target product nitrofurantoin.In the present embodiment, the total yield of the nitrofurantoin is about 70%. |
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