Related Products of 1891-90-3, A common heterocyclic compound, 1891-90-3, name is 4-(Trifluoromethyl)benzamide, molecular formula is C8H6F3NO, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.
First access in the microchannel reactor15 minutes of nitrogen replacement system air,Under full nitrogen protection conditions,Cool down at -30~-25C and start to join.95.5 g (0.5 mol, 99%)P-trifluoromethylbenzamide and 500a mixture of milliliters of methyl tert-butyl ether,At the same time, 0.323 liter (0.55 mol, 1.7 mol/L) was added dropwise.Tert-butyl lithium solution,The reaction solution is all introduced into a cryogenic collector to obtain a compound (III);Compound (III) and 66.1 g (0.6 mol, 99%) were then metered with a metering pump.The methyl methanesulfonate is kept between -30 and -25 C.Finished through the microchannel reactor for 1.5 hours,After the addition, the sample analysis did not detect trifluoromethylbenzamide.The reaction solution is slowly added to the person under nitrogen protection conditions.In ice water between 0-5 C,The solvent is removed by distillation under reduced pressure to give a yellow solid;Nuclear magnetic confirmation as the target product2-Methylsulfonyl-4-trifluoromethylbenzamide.The amount is 132 grams,97.8%,The yield was 96.7%.
The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.
Reference:
Patent; Papanna (Beijing) Technology Co., Ltd.; Xing Wenlong; Fu Renji; (7 pag.)CN109705005; (2019); A;,
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