Application of 3118-68-1, These common heterocyclic compound, 3118-68-1, name is 3-Cyanobenzenesulfonamide, 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.
The intermediate from step A above (722 mg), di-tert-butyl dicarbonate (1.6 g) and nickel(II) chloride hexahydrate (80 mg) was dissolved in dry methanol (20 mL) and cooled to 0 C. Then sodium borohydride (1.0 g) was added in portions and the ice bath removed. The mixture was vigorously stirred for 2 h, then diethylenetriamine (300 muL) was added and the mixture was concentrated to dryness. The residue was diluted with ethyl acetate, washed with 10% citric acid, saturated sodium hydrogen carbonate and brine, dried (MgSO4) and concentrated. Purification by column chromatography (dichloromethane/methanol, 96:4 to 95:5) gave a amorphous mass, which was suspended in hydrogen chloride (4M solution in dioxane, 15 mL) and stirred for 6 h, evaporated, slurried in diethyl ether and filtered to afford the title compound (590 mg; 67%). [M-Cl]+=187.
The synthetic route of 3118-68-1 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; Alantos Pharmaceuticals, Inc.,; US2006/173183; (2006); A1;,
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