4,6-Dinitro-2-sec-butylphenol synthesis

Yield:88-85-7 92.9%

Reaction Conditions:

with nitric acid at 40; under 4560.31 Torr; for 7 h;Autoclave;Inert atmosphere;Temperature;

Steps:

1-8 Example 7
After the reaction of Examples 5-6, the remaining spent acid is recovered and combined.A total of 313.6g, titrated acid concentration of 7.3%,Add 65% nitric acid to make 40% nitric acid.In a 500mL autoclave,Adding 212.53 g (1.35 mol) of 40% nitric acid,75.11g (0.5mol) of o-sec-butylphenol was added along the inner wall of the autoclave, and the autoclave was tightened.Nitrogen 6 atm test leak. Pass the condensed water, circulate internally, and start stirring.When the temperature in the kettle was down, heating was started and the temperature was set to 40 °C.After reaching the temperature, the reaction was kept for 7 h. When the pressure exceeds 10 kg/cm2, the pressure is released to 6 kg/cm2.After the reaction is completed, the condensed water is turned on to lower the temperature in the kettle.The kettle was opened, and the liquid in the kettle was taken into a separatory funnel and liquid was separated.Orange red liquid 111.8g(Yield: 92.9%, DNBP content 99.7%,2-sec-butylphenyl hydrazine content 0.3%);The water layer is 159.5g,The acid concentration was titrated to 9.82%.

References:

Dalian University of Technology;Gao Xinqin;Han Shangjie;Hou Wubeiwen;Wang Xiao;Li Huaqing CN110015961, 2019, A Location in patent:Paragraph 0052-0080

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