A method for synthesizing 5-chloro-2-methyl-4-(trifluoromethyl)aniline in one step
A trifluoromethyl, synthesis method technology, applied in the direction of preparation of amino compounds from amines, purification/separation of amino compounds, organic chemistry, etc., to achieve the effects of high yield, reasonable design, and simple operation
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[0018] A method for synthesizing 5-chloro-2-methyl-4-(trifluoromethyl)aniline in one step, the synthesis method comprises the following steps: according to the mass ratio of compound A, compound B, catalyst and carbonate is 50~ 55:45~50:5~10:45~47, the solid-liquid g / mL ratio of compound A and dioxane is 1:30, the raw materials are taken, and then compound A, catalyst and dioxane are mixed under nitrogen protection Put oxyhexane into the reactor, stir for 5 minutes, then add compound B and carbonate, raise the temperature to 100-105°C, and stir for 15-20 hours to obtain compound C, which is 5-chloro-2-methyl- 4-(Trifluoromethyl)aniline.
[0019] The chemical reaction formula of this synthesis is as follows
[0020] .
Embodiment 1
[0022] The catalyst is Pd(Dppf)Cl 2 .
[0023] The carbonate is any one of sodium carbonate and potassium carbonate.
[0024] A method for synthesizing 5-chloro-2-methyl-4-(trifluoromethyl)aniline in one step, the synthetic method comprises the following steps: under nitrogen protection, 5g compound A, 0.5g catalyst and 150mL dioxane Put the ring into the reactor, stir for 5min, then add 4.5g of compound B and 4.5g of carbonate, heat up to 100°C, stir and react for 15h, HPLC detects that the reaction of the raw materials is complete, the reaction solution is filtered through diatomaceous earth, concentrated, and the sample is mixed , 2.8 g of brown oil was obtained by passing through the column, that is, compound C, namely 5-chloro-2-methyl-4-(trifluoromethyl)aniline, with a yield of 85.9% and a purity of 99.1%.
[0025] The chemical reaction formula of this synthesis is as follows
[0026] .
[0027] NMR of 5-chloro-2-methyl-4-(trifluoromethyl)aniline: 1H NMR (d6-DMSO):...
Embodiment 2
[0029] The catalyst is Pd(Dppf)Cl 2 .
[0030] The carbonate is any one of sodium carbonate and potassium carbonate.
[0031] A method for synthesizing 5-chloro-2-methyl-4-(trifluoromethyl)aniline in one step, the synthetic method comprises the following steps: under nitrogen protection, 5g compound A, 0.8g catalyst and 150mL dioxane Put the ring into the reactor, stir for 5min, then add 4.8g of compound B and 4.6g of carbonate, heat up to 103°C, stir and react for 17h, HPLC detects that the reaction of the raw materials is complete, the reaction solution is filtered through diatomaceous earth, concentrated, and the sample is mixed , 3 g of brown oil was obtained by passing through the column, that is, compound C, namely 5-chloro-2-methyl-4-(trifluoromethyl)aniline, with a yield of 92.0% and a purity of 99.6%.
[0032] The chemical reaction formula of this synthesis is as follows
[0033] .
[0034] NMR of 5-chloro-2-methyl-4-(trifluoromethyl)aniline: 1H NMR (d6-DMSO): 7...
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