Synthetic Route of 108-70-3, A common heterocyclic compound, 108-70-3, name is 1,3,5-Trichlorobenzene, molecular formula is C6H3Cl3, 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.
A 50 mL 3 neck round bottom flask was oven dried, cooled under nitrogen, and char- ged with 14.50 g of xylenes. The flask was then charged with 1,3, 5-TRICHLOROBENZENE (9.760g, 53.49 MMOL), benzophenone imine (7.620 g, 42.04 MMOL), (dba) 3PD2 CATALYST (0.023 g, 0.03 mmol in 2 g xylene), dppf ligand (0.042 g, 0.08 MMOL IN 2 G XYLENE) and sodium t-butoxid (5.550 g, 57.70 mmol). The reaction mixture was heated to reflux (136 C) for 3 hours and then cooled to room temperature. The aromatic imine intermediate was then hydrolyzed with 22 ML OF 2 N HCI (aq) at 70 C for 45 minutes. The hydrochloride salt of dichloroaniline precipitated out of solution when cooled to room temperature. The crude hydrochloride salt was collected by filtration using a buchner funnel and then washed with methyl-tert. butyl ether. The DICHLOROANALINE SALT was then added to 30 mL of METHYL-TERT. BUTYL ether and pH adjusted to 12 using 50% NaOH. The methyl-tert. butyl ether phase was collected and then stripped under va- cuum to give 3, 5-DICHLOROANILINE in 86 % yield.
The synthetic route of 108-70-3 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; BASF AKTIENGESELLSCHAFT; WO2004/54961; (2004); A1;,
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