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ChemicalBook CAS DataBase List 2,5-Dichloronitrobenzene
89-61-2

2,5-Dichloronitrobenzene synthesis

13synthesis methods
Nitration of 1,4-dichlorobenzene with mixed acid at 35 – 65 ℃ results in a 98 % yield of essentially pure 2,5-Dichloronitrobenzene.
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Yield:89-61-2 96.7%

Reaction Conditions:

with ortho-difluorobenzene;sulfuric acid;nitric acid at 35;Temperature;

Steps:

1.1; 1.2; 1.3 Example 1
(1) Dissolve 300 g of 1,4-dichlorobenzene in 2 L of methylene chloride as material 1 and measure 400 ml of concentrated nitric oxide.Acid as the material 2, the amount of 600mL concentrated sulfuric acid as material 3;(2) The flow rate of the control material 1 is 15 ml/min; the flow rate of the control material 2 is 8 min/min; the flow of the control material 3 isThe speed is 12min/min; the reaction temperature is 35°C,The molar ratio of o-difluorobenzene to nitric acid is 1:2.5;The molar ratio of nitric acid to concentrated sulfuric acid is 1:2.0; the residence time of the reaction is 70s;(3) After each stock in the reactor reaches a steady state, collect the reaction liquid from the outlet of the reactor to passThe reaction solution corresponding to the material 1 (ie, 1800 ml of material 1, 260.0 g of 1,4-dichlorobenzene) for 120 min was taken as an example. The liquid and organic phases were retained, and the acid layer was extracted once with 500 ml of dichloromethane, and the organic phases were combined. After adding 500ml of 10% Na2CO3 to wash once, drying and then removing the organic solvent under reduced pressure, and then distilling to obtain the first step nitration product 2,5-dichloronitrobenzene 328.4g, the yield of 96.7%, liquid phase Purity 99.6%.

References:

Heilongjiang Xinchuang Bio-technology Development Co., Ltd.;Liu Guimei;Ren Jiqiu;Yang Kun;An Yongsheng CN106565500, 2017, A Location in patent:Paragraph 0041; 0042; 0051; 0052; 0053; 0054; 0060; 0061

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