N-NITROSODIACETONITRILE synthesis

Yield:16339-18-7 95%

Reaction Conditions:

with sulfuric acid;sodium nitrite in water at 0 - 30; for 2.5 h;Temperature;

Steps:

1; 2; 3; 4; 5; 6; 7; 8; 9 Example 1

The control temperature is between 0 ° C and 5 ° C.900 g of 20% by mass sulfuric acid (1.84 moL) and 200 g (2.1 moL) of iminodiacetonitrile were added to a 3 L three-neck round bottom flask, and the mixture was sufficiently dissolved.A solution of 320 g (4.64 mol) of NaNO2 dissolved in 900 g of water was added dropwise.After the addition of 2h, the control temperature was reacted at 30 ° C for 0.5 h.The reaction mixture was extracted 3 times with 2000 mL of ethyl acetate.The organic phases were combined, washed with water until neutral, dried over anhydrous MgSO4.Evaporate the solvent,A pale yellow solid of 248.0 g was obtained with a purity of 99.6% and a yield of 95%.

References:

CN110156636,2019,A Location in patent:Paragraph 0013-0037