ChemicalBook CAS DataBase List 2,3-DIMETHYL-2,3-DINITROBUTANE

2,3-DIMETHYL-2,3-DINITROBUTANE synthesis

12synthesis methods

Product Name:2,3-DIMETHYL-2,3-DINITROBUTANE
CAS Number:3964-18-9
Molecular formula:C6H12N2O4
Molecular Weight:176.17

The synthesis of 2,3-dimethyl-2,3-dinitrobutane is as follows:

Add 4.5 g (0.05 mol) of 2-nitropropane and 9 mL of a 6 mol/L sodium hydroxide solution to a 100 mL three-necked flask. The reaction was stirred magnetically for 0.5 h in an ice-water bath, and 4 g (0.025 mol) of liquid bromine was added dropwise to the flask using a constant pressure dropping funnel. After the dropwise addition was completed, 15 mL of absolute ethanol was added to thereto, and stirring was continued in an ice bath for 0.5 h. Then the ice bath was removed, the temperature was raised to 90℃, and the reaction was refluxed for 2 hours to stop the reaction. After the reaction liquid was naturally cooled to room temperature, a large amount of white solid precipitated, filtered, washed several times with absolute ethanol and distilled water, and dried under vacuum to obtain 40.13 g of white flake crystals. The yield was 91.2%.

79-46-9 Synthesis

79-46-9
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3964-18-9
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Yield:3964-18-9 91.2%

Reaction Conditions:

Stage #1: 2-nitropropanewith sodium hydroxide for 0.5 h;Cooling with ice;
Stage #2: with bromine in ethanol at 90; for 2.5 h;Cooling with ice;

Steps:

1-2 Example 1

Add 4.5 g (0.05 mol) of 2-nitropropane and 9 mL of a 6 mol / L sodium hydroxide solution to a 100 mL three-necked flask.The reaction was stirred magnetically for 0.5 h in an ice-water bath, and 4 g (0.025 mol) of liquid bromine was added dropwise to the flask using a constant pressure dropping funnel.After the dropwise addition was completed, 15 mL of absolute ethanol was added thereto, and stirring was continued in an ice bath for 0.5 h.Then the ice bath was removed, the temperature was raised to 90 ° C, and the reaction was refluxed for 2 hours to stop the reaction. After the reaction liquid was naturally cooled to room temperature,A large amount of white solid precipitated, filtered, washed several times with absolute ethanol and distilled water, and dried under vacuum to obtain 40.13 g of white flake crystalsThe yield was 91.2%. This product was 2,3-dimethyl-2,3-dinitrobutane.

References:

CN110818638,2020,A Location in patent:Paragraph 0034-0035; 0044-0045

127-06-0 Synthesis