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ChemicalBook CAS DataBase List 2-Cyanoacetamide
107-91-5

2-Cyanoacetamide synthesis

12synthesis methods
Cyanoacetamide can be prepared from ethyl cyanoacetate and ammonia. Cool the ethyl cyanoacetate to below 200°C, add concentrated ammonia water to react, and the mixture turns from turbid to clear. After cooling in cold water for 20 minutes, a precipitate is precipitated. After filtration and drying, the crude product is obtained, and then the crude product of cyanoacetamide is added. In the boiling ethanol, after dissolving it, add a small amount of activated carbon for decolorization and purification, filter, cool the filtrate to separate out the precipitate, and dry it at 80-100 ℃ to obtain the fine cyanoacetamide.
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Yield:107-91-5 99%

Reaction Conditions:

with bis(trichloromethyl) carbonate in cyclohexane at 80; under 11251.1 Torr; for 0.5 h;Pressure;Solvent;Temperature;

Steps:

1-5 Example 2

Weigh 112.3g (1.1mol) of malonamide,Stir 377.1g of cyclohexane in a mixing bottle evenly,The temperature of the pipeline reactor is set to 80, the pressure is 1.5MPa,The flow rate of pump A is set to 2ml/min, and the flow rate of pump B is set to 2ml/min.After reaching the set temperature, open the exhaust gas exhaust valve and the triphosgene solution dripping valve,Turn on pump A and feed the cyclohexane solution of malonamide, turn on pump B and feed the cyclohexane solution of triphosgene (297g triphosgene is dissolved in 891ml cyclohexane). After 30 minutes, take a sample to detect the moisture content of the reaction solution at the outlet of the reactor. 0.2%. After the sample is injected, the reaction solution in the receiving bottle is subjected to atmospheric distillation to recover cyclohexane and a small amount of residual raw materials. The end temperature of the rectification is 80, and then the temperature is lowered and centrifuged to obtain 93.2g of cyanoacetamide, which is cyanoacetamide Detected by HPLC, the purity is calculated by the external standard method: 98.3%, and the yield is 99.0%.

References:

CN113292452,2021,A Location in patent:Paragraph 0021-0030

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