[NH3:1].[C:2]([CH2:4]C(OCC)=O)#[N:3].[N:10]([O-])=O.[Na+].S(=O)(=O)(O)O.[C:19](=[O:22])([O-])[O-].[K+].[K+].S([O:30][CH3:31])(OC)(=O)=O>O>[C:4]([C:2](=[N:3][O:22][CH3:19])[C:31]([NH2:10])=[O:30])#[N:1]To a solution of an aqueous concentrated ammonia (64.5 g, 1.07 mol) in water (28.7 ml), ethyl cyanoacetate (100 g, 0.89 mol) was added dropwise at -5° C. under ice-cooling. After completion of the reaction, the mixture was concentrated under reduced pressure. A solution of sodium nitrite (73.3 g, 1.06 mol) in water (151 g) was added to the residue. The mixture was maintained at an internal temperature of 38° to 48° C., to which 62.5% sulfuric acid (76.3 g, 0.49 mol) was added dropwise. After completion of the addition, the mixture was stirred at the same temperature for 1 hr, and then potassium carbonate (73.3 g, 0.53 mol) in water (110 g) was added dropwise followed by dimethyl sulfate (133.8 g, 1.06 mol) at 38° to 48° C. The mixture was stirred at the same temperature for 1 hr. and cooled. The resulting crystals were washed with water (150 ml) at 50° C., filtered and dried to give 2-cyano-2-methoxyimino-acetamide (92.2 g, yield: 82%).
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