DISODIUM CYANAMIDE synthesis
- Product Name:DISODIUM CYANAMIDE
- CAS Number:20611-81-8
- Molecular formula:CN2Na2
- Molecular Weight:86
156-62-7
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Yield:-
Reaction Conditions:
with sodium hydroxide in water at 25; for 1 h;
Steps:
Synthesis of N,N-bis(3,3-dimethyl-allyl)-cyanamide
3,3-dimethyl-diallyl-cyanamide was synthesised according to the method reported by E. B. Vliet [26] , but with slight modifi- cation. In a two-necked round bottom flask fitted with a reflux condenser and mechanical stirrer, about 90 mL water and 18 g of cracked ice were introduced. To this mixture 27.5 g (0.44 mol) of fresh cyanamide was added slowly with continuous stirring. Af- ter suspending all the cyanamide in water, a cold solution of 15 g (0.38 mol) sodium hydroxide in 30 mL water was added and vigor- ous stirring of the mixture was maintained for 1 h while maintain- ing the temperature under 25 °C by the addition of ice at differ- ent intervals. Then, to the prepared solution of sodium cyanamide, 100 mL ethanol (95%) was added, followed by dropwise addition of 62 g (0.42 mol) of 3,3 dimethyl-allyl-bromide. The mixture was thereafter heated gently to refluxing temperature on a water bath while maintaining steady stirring 2.5 h. At the end, the ethanol in excess is removed by distillation. Yield: 6.84 g, 18.32%; Selected IR data (solid ATR, cm -1 ): 3489 w, 2972s, 2928s, 2209s, 1616 m, 1571 m, 1448s, 1318 m, 1277 w, 1028 w, 773 m; 1 H NMR (300 MHz, CDCl 3 , ppm, J Hz): 5.27 (t, 2H, H 2 , J = 7.4), 3.55 (d, 4H, H 1 , J = 7.4), 1.78 (s, 6H, H 5 ), 1.67 (s, 6H, H 5 ); 13 C{ 1 H}-NMR (75 MHz, CDCl 3 , ppm): 139.56 (C 2 ); 118.46 ( C N), 117.60 (C 3 ), 48.26 (C 1 ), 25.89 (C 4 ), 18.09 (C 5 ).
References:
Badiceanu, Carmellina Daniela;Bartha, Emeric;Draghici, Constantin;Ekennia, Anthony C.;Hrubaru, Madalina M.;Okafor, Sunday N.;Onwudiwe, Damian C.;Shova, Sergiu;Udu, David Agwu [Journal of Molecular Structure,2022,vol. 1250,art. no. 131649]
178560-14-0
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64-17-5
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74-86-2
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71-43-2
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