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ChemicalBook CAS DataBase List 1,2,3-Trifluoro-4-nitrobenzene

1,2,3-Trifluoro-4-nitrobenzene synthesis

11synthesis methods
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Yield:771-69-7 85.5%

Reaction Conditions:

Stage #1:1,3-dichloro-2-fluorobenzene with sulfuric acid;nitric acid at 20 - 25; for 2.5 h;
Stage #2: with sulfolane;potassium fluoride for 5 h;

Steps:

10 Example 10
n a 250 ml four-necked flask, 64 g of 98% concentrated sulfuric acid was charged(0.606 mol) of 2,6-dichlorofluorobenzene was added dropwise to a stirred solution of 33 g of 98% concentrated sulfuric acid at 20 to 25 ° CMixed with 39 g of 98% concentrated nitric acid, 2.5 hThe addition is complete.After warming up to 40 ~ 45 ° C and heat 1.5 hours. After the end of the washing, to neutral, organic subtractionPressure dehydration after use.In a 250 ml four-necked flask285gSulfolane and87g (1.5mol) KF, after dehydration by adding the last step nitration products,In 195 ± 5 ° C heat 5h, vacuum distillation of the solvent and then distillation 2,3,4-trifluoronitrobenzene 91. 7g,The content was 99.8% and the yield was 85.5%

References:

Binhai Yongtai Medical Chemical Co Ltd;He, Renbao;Shao, Hongming CN102249881, 2016, B Location in patent:Paragraph 0015; 0057-0059

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