80194-70-3Relevant articles and documents
Combined preparation method of 2-cyano-3-chloro-5-trifluoromethylpyridine and succinonitrile
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Paragraph 0024-0036, (2021/02/24)
The invention discloses a combined preparation method of 2-cyano-3-chloro-5-trifluoromethylpyridine and succinonitrile, and belongs to the field of organic chemistry. The method comprises the following steps: taking 2-fluoro-3-chloro-5-trifluoromethylpyridine and dichloroethane as raw materials, reacting in a potassium cyanide/sodium solution under the action of a phase transfer catalyst to obtaina mixed solution of 2-cyano-3-chloro-5-trifluoromethylpyridine and succinonitrile, layering, washing with water, and rectifying to obtain the 2-cyano-3-chloro-5-trifluoromethylpyridine with the content of more than 99% and the succinonitrile with the content of more than 99.9%. According to the method, the yield is high, the wastewater treatment is simple, byproducts are fully utilized, the yieldof the 2-cyano-3-chloro-5-trifluoromethylpyridine can reach 93%, and the yield of the succinonitrile can reach 95%.
3-chloro-2-cyano-5-trifluoromethyl pyridine preparation method
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Paragraph 0025, (2017/04/28)
The invention discloses a 3-chloro-2-cyano-5-trifluoromethyl pyridine preparation method. The method includes steps: (1) dissolving 3-chloro-2-R-5-trifluoromethyl pyridine into a solvent A, adding an activating agent, performing heating reflux for 4-6h, cooling to 20-30 DEG C to obtain reaction liquid, filtering the reaction liquid to obtain a filter cake, and subjecting the filter cake to vacuum drying for 1-2h at 40-50 DEG C to obtain organic salt; (2) adding cyanide and the organic salt obtained at the step (1) into a solvent B and water, stirring for reaction for 2-3h at 0-80 DEG C to obtain mixed liquid, and standing the mixed liquid for layering to obtain an organic phase a; adding hydrochloric acid into the organic phase a to adjust pH to 2-4, standing for layering to obtain an acid water layer and an organic layer, and adding water to wash the organic layer until pH is 6-7, so that washed water and an organic phase b are obtained. By the preparation process, nitrile solvents such as acetonitrile and propionitrile are avoided while low-toxicity solvents such as dichloromethane hardly soluble in water are adopted, conception ingenuity is achieved, solvent recycling is realized, and accordingly production cost is reduced, and environment pollution is abated.
Homogenous suspension of immunopotentiating compounds and uses thereof
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, (2016/09/12)
The present invention generally relates to homogeneous suspensions of small molecule immune potentiators (SMIPs) that are capable of stimulating or modulating an immune response in a subject in need thereof. The homogeneous suspensions may be used in combinations with various antigens or adjuvants for vaccine therapies.