Cyanamide → HCID 86643043, compound
Reaction equation
[N:1]#[C:2][NH2:3].C[O-].[Na+:6].C(O[C:10](=[C:13]([C:16]#[N:17])[C:14]#[N:15])[CH2:11][CH3:12])C>C(O)C>[C:2]([N-:3][C:10](=[C:13]([C:16]#[N:17])[C:14]#[N:15])[CH2:11][CH3:12])#[N:1].[Na+:6]Participants
5
Reactant 3
Product 1
Reagents, catalysts & solvents 1
Conditions
- Temperature
- 25 °C
Procedure
In portions, 7.56 g of cyanamide are added to a solution of 32.38 g (33.4 ml, density=0.97 g/l) of 30% sodium methanolate solution and 100 ml of ethanol and the mixture is stirred at 25° C. for ca. 5 minutes; then, over the course of ca. 25 minutes, 30 g (ca. 90% strength, 180 mmol) of (1-ethoxypropylidene)malononitrile are added dropwise. The mixture is stirred for two hours, then the volatile constituents are largely removed by distillation, and the remaining residue is taken up in methylene chloride. The methylene chloride phase is separated off and the remaining 37.57 g of sodium cyano[1-(dicyanomethylidene)propyl]azanide with ca. 80% purity are used in the following stage.
Workup
- stirringThe mixture is stirred for two hours
- customthe volatile constituents are largely removed by distillation
- customThe methylene chloride phase is separated off
Sources & evidence
- ORD record
- ord-39e2114d5f9743aa963bd1eb88803c6f
- Source dataset
- uspto-grants-2012_12
- Patent number
- US08329717B2
Reaction notes
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