Welcome to chemicalbook!
Chinese English Japanese Germany Korea
400-158-6606
Try our best to find the right business for you.
Do not miss inquiry messages Please log in to view all inquiry messages.

Welcome back!

ChemicalBook CAS DataBase List DISODIUM CYANAMIDE

DISODIUM CYANAMIDE synthesis

6synthesis methods
-

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]