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ChemicalBook CAS DataBase List Cyanamide
420-04-2

Cyanamide synthesis

10synthesis methods
The basic process for the manufacture of cyanamide comprises four steps. The first three steps produce calcium cyanamide: lime is made from high grade limestone; (2) calcium carbide is manufactured from lime and coal or coke; calcium cyanamide is produced by passing gaseous nitrogen through a bed of calcium carbide with 1% calcium fluorspar, which is heated to 1000–1100°C to start the reaction—the heat source is then removed and the reaction continues because of its strong exothermic character; and cyanamide is manufactured from calcium cyanamide by continuous carbonation in an aqueous medium.
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Yield:420-04-2 12 %Spectr.

Reaction Conditions:

in tert-butyl methyl ether at 40; for 2 h;

Steps:

1 Example 1

Example 1 A reactor was charged with 75 g of methyl tert-butylether, after which gaseous cyanogen chloride and gaseous ammonia were fed to the solution, keeping the temperature below [40°C] by cooling. After 2 h the precipitate (ammonium chloride) was removed by filtration and a clear solution was obtained which was stripped with nitrogen and which contained 12% of pure cyanamide (determined by Raman spectroscopy). 55 g of the thus obtained organic solution (containing 6.6 g of cyanamide) were directly dosed within 3 h to 71 g of an aqueous solution containing 20.4 g of sodium sarcosinate, keeping the temperature at [50°C] and the pH at 9.8 by addition of formic acid. After continuing stirring for another 1 h at [50°C,] the white precipitate formed was filtered, washed with water, and dried. 16.5 g (70% yield) of creatine monohydrate were obtained with a purity > [99%] according to HPLC analysis.

References:

WO2004/31133,2004,A1 Location in patent:Page 3

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