Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 654-70-6, name is 4-Cyano-3-trifluoromethylaniline, A new synthetic method of this compound is introduced below., category: nitriles-buliding-blocks
Compound R-III (6.00 g, 32.9 mmol),4-cyano-3-trifluoromethylaniline (6.79 g, 36.5 mmol)Add N,N-methylacetamide (42 mL) to the reaction flask and cool to -15 C in an ice bath.Thionyl chloride (4.60 g, 39.0 mmol) was added dropwise, and the reaction temperature was controlled from -10 C to -15 C.After the dropwise addition was completed, the mixture was stirred for 0.5 h, and then raised to 40 C for 3 h.The reaction was slowly poured into cold saturated sodium bicarbonate solution (120 mL).Extract with ethyl acetate (30 mL x 3), combine the organic phases and wash with saturated sodium chloride.Filtration and evaporation of the solvent under reduced pressure afforded crude material.Recrystallization from a mixed solution of petroleum ether and methyl tert-butyl ether, decolorization of activated carbon,Obtained white solid R-IV 9.30g, yield 80.4%,
The synthetic route of 654-70-6 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; Shijiazhuang Du Zhi Pharmaceutical Technology Co., Ltd.; Fang Yu; Du Yumin; (10 pag.)CN109761778; (2019); A;,
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