Synthetic Route of 210532-25-5, These common heterocyclic compound, 210532-25-5, name is 3,5-Difluorobenzene-1-sulfonyl chloride, 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.
To a stirred suspension of TFA salt of 9-(3-amino-propyl)-6,7,8,9-tetrahydro-5H- carbazole-3-carboxylic acid methyl ester (0.2 g, 0.5 mmol), in 2 ml of dry CH2Cl2, NEt3 (0.208 ml, 1.5 mmol) was added at 0 C. After stirring for 5 min, 3,5-difluorobenzene sulfonylchloride (0.106 g, 0.5 mmol), in 1 ml of dry CH2Cl2 was added and the mixture was stirred for 3 hrs. The reaction mixture was diluted with CH2Cl2, washed sequentially with IN HCl (25 ml), H2O (25 ml) and sat. NaHCO3 (25 ml) solution. The organic layer was separated, dried over anhyd.MgSO4, solvents removed in vacuo and the crude was purified by column chromatography, using EtOAc/hexane as eluents, to obtain 0.14g of the product. 1H NMR 500 MHz CDCl3: 8.2, d, J = 1.4, IH, 7.8, dd, J = 1.6, 8.7, IH, 7.3-7.24, m, 2H, 7.15, d, J = 8.7, IH, 7.04-6.97, m, IH, 4.48, t, J = 5.9, IH, 4.1, t, J = 7, 2H, 3.92, s, 3H, 2.98, q, J = 6.6, 2H, 2.73, t, J = 6.2, 2H, 2.66, t, J = 5.9, 2H, 2.05-1.89, m, 4H, 1.88-1.82, m, 2H.
The synthetic route of 210532-25-5 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; ITHERX PHARMACEUTICALS, INC.; WO2009/103022; (2009); A1;,
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