Synthetic method for 2-methyl-3-trifluoromethylaniline
A technology of trifluoromethylaniline and a synthesis method, which is applied in the preparation of amino compounds, chemical instruments and methods, preparation of amino compounds from amines, etc., can solve the problems of cumbersome experimental process and poor operability, and achieves easy handling and environmental protection pressure. Small, production-safe effect
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[0037] Example 1
[0038] 1. Synthesis of 6-chloro-2-(methylthio)methyl-3-trifluoromethylaniline:
[0039] Weigh 606.2g of 2-chloro-3-trifluoromethylaniline, add 4L of dichloroethane, stir evenly, add 280.2g of dimethyl sulfide and N-chlorosuccinimide to the system, and control the addition rate , Make the system temperature not higher than 30 degrees, after the addition, the system is stirred at room temperature for 6 hours, then 636g of triethylamine is added to the system, the system is heated to reflux, the temperature is lowered, water is added, the liquid is separated, the solvent is removed, and the residue is reduced Pressure distillation obtains 635.8 g of product, the yield is 80%, and the HPLC purity is greater than 97%. 1 H NMR(600MHz, CDCl 3 )δ7.304(d,J=8.4Hz,1H),7.016(d,J=8.4Hz,1H),5.2-4.7(br s,2H),3.885(s,2H),2.051(s,3H)
[0040] 2. Synthesis of 6-chloro-2-chloromethyl-3-trifluoromethylaniline hydrochloride:
[0041] Weigh 568.2g of 6-chloro-2-(methylthio)methyl-3-trif...
Example Embodiment
[0044] Example 2
[0045] 1. Synthesis of 6-chloro-2-(methylthio)methyl-3-trifluoromethylaniline:
[0046] Weigh 1170g of 2-chloro-3-trifluoromethylaniline, add 17L of dichloroethane, stir evenly, add 354g of dimethyl sulfide and 961g of N-chlorosuccinimide to the system, and control the addition rate. Keep the temperature of the system not higher than 30 degrees. After the addition, the system is stirred at room temperature for 6 hours, and 1214g of triethylamine is added to the system. The system is heated to reflux, the temperature is lowered, water is added, the liquids are separated, the solvent is removed, and the residue is reduced in pressure Distilled to obtain 1193 g of product, the yield was 78%, and the HPLC purity was greater than 95%. 1 H NMR(600MHz, CDCl 3 )δ7.304(d,J=8.4Hz,1H),7.016(d,J=8.4Hz,1H),5.2-4.7(br s,2H),3.885(s,2H),2.051(s,3H)
[0047] 2. Synthesis of 6-chloro-2-chloromethyl-3-trifluoromethylaniline hydrochloride:
[0048] Weigh 1020g of 6-chloro-2-(methylth...
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