solution of 2 92 g of n 330 dimethylamino 2 cyano 2 propen 1 ylidene n 39 n 39 n 39 trimethylhydrazinium methyl sulfate in 20 ml of methanol was added in small portions at room temperature 540 mg of sodium methoxide the resulting mixture was stirred at room temperature for 30 minutes then the solvent was evaporated under reduced pressure the residue was dissolved in hot water on cooling dimethylaminomethylenemalononitrile crystallized out and was collected by filtration m p 81 u00b0 83 u00b0 to a slurry of 12 4 g of 2 cyano 3 dimethylaminoacrolein in 50 ml of water was added in small portions 13 6 g of hydroxylamine 0 sulfonic acid 91 pure the resulting clear solution was stirred for an additional 10 minutes then cooled to 0 u00b0 and adjusted to ph 6 0 by addition of approximately 26 ml of 5n sodium hydroxide solution the mixture was heated for 20 minutes in a water bath at 70 u00b0 a ph 3 was maintained over this period by dropwise addition of 5n sodium hydroxide solution after cooling to room temperature the mixture was extracted with 3 u00d7 100 ml of methylene chloride the combined extracts were washed with 50 ml of water dried over magnesium sulfate filtered and evaporated to dryness under reduced pressure thus dimethylaminomethylenemalononitrile was obtained after recrystallization from isopropanol the material had a melting point of 93 u00b0 95 u00b0 into a 250 ml 3 neck round bottom flask are placed 7 3 g 0 1m of dimethylformamide and 150 ml of dichloromethane the stirred solution is cooled in ice water and phosgene is bubbled through for 30 minutes a white solid forms the solvent is removed under reduced pressure the.