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2-ethoxy-6-pentadecyl-benzoyl chloride was condensed with 4-Amino-2-trifluromethyl benzonitrile in dichloromethane in presence of triethylamine as acid scavenger to yield N-(4-Cyano-3-trifluoromethyl-phenyl)-2-ethoxy-benzamide. The reaction mixture was then concentrated in vacuo and the residue was extracted into ethyl acetate. The ethyl acetate layer was washed with water and with cold aqueous hydrochloric acid, then dried over sodium sulphate and finally concentrated in vacuo. The residue obtained was chromatographed over silica gel to afford the desired product. 1H-NMR:delta6.95-8.01 (7H,aromatic), delta3.98(2H,m,OCH2), delta1.33(3H,t,Methyl)
With sodium hydroxide; In N,N-dimethyl-formamide; at 20℃; for 5h;
0.30g (0.0075 mol) of sodium hydroxide was added to a solution of 0.7g(0.0037 mol) of 4-amino-2-(trifluoromethyl)benzonitrile in 40 mL of DMF, followed by addition of 1g (0.0037 mol) of <strong>[1897-41-2]2,3,5,6-<strong>[1897-41-2]tetrachloroterephthalonitrile</strong></strong> understirring, the mixture was stirred for 5 h after addition at room temperature. After the reaction was over by Thin-LayerChromatography monitoring, the reaction mixture was poured into water, solid precipitated and filtered under reducedpressure to give 1.3 g of compound C-38 as yellow solid, m.p. 176-178°C.[0117] 1H-NMR (300MHz, internal standard TMS, solvent CDCl3) delta(ppm): 6.86(dd, 1H, Ph-6-1H),7.16 (d, 1H, Ph-2-1H), 7.73 (d, 1H, Ph-5-1H).
1.3 g
With sodium hydroxide; In N,N-dimethyl-formamide; at 20℃; for 5h;
0.30 g (0.0075 mol) of sodium hydroxide was added to a solution of 0.7 g (0.0037 mol) of 4-amino-2-(trifluoromethyl)benzonitrile in 40 mL of DMF, followed by addition of 1 g (0.0037 mol) of <strong>[1897-41-2]2,3,5,6-<strong>[1897-41-2]tetrachloroterephthalonitrile</strong></strong> under stirring, the mixture was stirred for 5 h after addition at room temperature. After the reaction was over by Thin-Layer Chromatography monitoring, the reaction mixture was poured into water, solid precipitated and filtered under reduced pressure to give 1.3 g of compound C-38 as yellow solid, m.p. 176-178° C. [0182] 1H-NMR (300 MHz, internal standard TMS, solvent CDCl3) delta (ppm): 6.86 (dd, 1H, Ph-6-1H), 7.16 (d, 1H, Ph-2-1H), 7.73 (d, 1H, Ph-5-1H).
With hydrogenchloride; copper(l) iodide; thionyl chloride; sodium nitrite; In water; acetone; at 0 - 20℃; for 1.0h;
Anhydrous cuprous chloride (0.3 g, 0.003 mol, 0.011 eq.) Was added to 500 ml of water, and 80 ml of dichlorosulfoxide was added dropwise under an ice-water bath, and rt overnight to obtain solution a;4-amino-2- (trifluoromethyl) benzonitrile (50.0 g, 0.269 mol, 1.0 eq.)Add 260ml of concentrated hydrochloric acid and 50ml of acetone in an ice water bath.Add sodium nitrite (20.4g, 0.296mol,1.1eq.) Dissolved in 20ml of water, stirred at 0 C for 30min,Get reaction solution a;Then add the reaction solution a dropwise to the solution a, and react at room temperature for 30 minutes.TLC monitors for complete response.
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