Methane, dinitro-,ion(1-), sodium (8CI,9CI) synthesis

Yield:25854-41-5 77%

Reaction Conditions:

with nitromethane;sodium hydroxide in methanol at 0 - 5; for 1 h;

Steps:

Dinitromethane Sodium Salt 22

CAUTION Although we encountered no difficulties during the prepa-ration and handling of dinitromethane sodium salt, it is a potentiallyexplosive energetic material which is sensitive to impact and friction.Mechanical actions of this energetic material, involving scratching orscraping, must be avoided. Any manipulations must be carried out byusing appropriate standard safety precautions.Tetranitromethane (60 mL, 0.5 mol) was added to a solution of nitro-methane (27 mL, 0.5 mol) in MeOH (150 mL) at room temperatureand under mechanical stirring. The reaction mixture was cooled to -5 °C (dry ice bath) and a cold solution of NaOH (40 g, 1.0 mol) inMeOH (500 mL) was added dropwise. After the addition was com-plete, the mixture was stirred for 1 h at 0 °C. The solid was filtered offand washed with acetone (6 × 50 mL) and Et 2 O (2 × 50 mL). The prod-uct was dried in air as a thin layer for 40 min and kept in a freezer. Theobtained dinitromethane sodium salt can be stored at -20 °C for atleast 4 months without decomposition.Yield 49.3 g (77%).

References:

Fershtat, Leonid L.;Bystrov, Dmitry M.;Zhilin, Egor S.;Makhova, Nina N. [Synthesis,2019,vol. 51,# 3,p. 747 - 756]