Introduction of a new synthetic route about 90357-53-2

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.

Electric Literature of 90357-53-2, A common heterocyclic compound, 90357-53-2, name is N-(4-Cyano-3-(trifluoromethyl)phenyl)methacrylamide, molecular formula is C12H9F3N2O, 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.

Example 29; S-r¡ã-Fluoro-phenvO-S-methYl-S^-dihydro-SigmaH-pyrazole-S-carboxylic acidM-cvano-S-trifluoromethyl-PhenvD-amide and S-r¡ã-Fluoro-phenvO-S-methvM.S-dihvdro-SH-pyrazole-S-carboxylic acid r¡ã-cvano-S-trifluoromethyl-phenvQ-amide; Compound No.1 and Compound No.64; 2-[(1 E)-(4fluorophenyl)methylidene] toluenesulfonylhydrazone, prepared according to the procedure described in Example 29 (600 mg, 2.1 mmol) in THF (20 ml) was treated by NaH (60%, 120 mg, 3 mmol) at 0C for 20 min, followed by the addition of N-(4-cyano-3-trifluoromethyl-phenyl)-2-methyl- acrylamide (500 mg, 2.0 mmol). The reaction mixture was then heated to 55C overnight, then quenched by NaHCO3, and extracted by ethyl acetate. The organic layer was combined, washed with brine, dried over Na2SO4 and concentrated to yield crude product as a mixture. Purification of the crude product on a column yielded the title compound as separate products, as a white solids.5-(4-Fluorophihenyl)-3-methyl-3,4-dhydro-2H-pyrazole-3-carboxylic acid (4-cyano-3-trifluoromethyl-phenyl)-amide (Hexane: ethyl acetate, 2:1 , Rf= 0.45, 475 mg, 61 %)5-(4-Fluoro-phenyl)-3-methyl-4,5-dihydro-3H-pyrazole-3-carboxylic acid (4-cyano-3-trifluoromethyl-phenyl)-amide(Hexane: ethyl acetate: 2:1 , Rf=0.6, 100 mg, 13%): MS (m/z): MH+ (391) EPO 1H NMR (CDCI3) delta 8.50 (s, 1 H), 8.10 (s, 1 H), 7.90 (del, J=1.5 Hz, 0.2 Hz, 1 H), 7.75 (d, J=1.5 Hz, 1 H), 7.20 (m, 2H), 7.10 (m, 2H), 5.60 (t, J=0.9 Hz, 1 H), 3.00 (dd, J=1.0 Hz, 0.8 Hz, 1 H), 1.87 (s, 3H), 1.55 (t, J=1.1 Hz, 0.6 Hz, 1 H).

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; JANSSEN PHARMACEUTICA N.V.; WO2006/55184; (2006); A2;,
Nitrile – Wikipedia,
Nitriles – Chemistry LibreTexts