Related Products of 654-70-6,Some common heterocyclic compound, 654-70-6, name is 4-Cyano-3-trifluoromethylaniline, molecular formula is C8H5F3N2, 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.
Step 22.3: 4-Amino-2-trifluoromethyl-benzaldehyde A solution of 3 g (0.0161 mol) 4-amino-2-trifluoromethyl-benzonitrile in 9 mL of dry THF is treated dropwise at rt and under nitrogen with 26.85 mL (0.0403 mol) of a 1.5 M diisobutyl-aluminum-hydride solution in toluene. During the addition the temperature is maintained at maximally 28 C. by appropriate cooling. After complete addition the brown solution is allowed to stand at rt over night. It is then added dropwise to a mixture of 4.4 mL of methanol and 39 mL of a saturated (~3M) potassium sodium tartrate solution. During the hydrolysis the temperature is kept below 40 C. After stirring for 15 minutes ethyl acetate is added and the two layers separated. The ethyl acetate phase is washed with water and brine, dried with sodium sulphate and evaporated. The brown foam obtained consists of oligomeric forms of the aldehyde (imine formation) and is therefore re-dissolved in 10 mL of ethyl acetate and stirred efficiently for 10 minutes with 10 mL of 1 N HCl. Sodium hydroxide (1 N, 8.5 mL) is added and stirring is continued for 5 more minutes (at the end the solution has pH ~9). The ethyl acetate is separated, washed with brine, dried with sodium sulphate and evaporated to give crude 4-amino-2-trifluoromethyl-benzaldehyde as a brown oil which is immediately used in the next step.
The synthetic route of 654-70-6 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; Caravatti, Giorgio; Furet, Pascal; Imbach, Patricia; Martiny-Baron, Georg; Perez, Lawrence Blas; Sheng, Tao; US2006/35897; (2006); A1;,
Nitrile – Wikipedia,
Nitriles – Chemistry LibreTexts