Reference of 53297-68-0, A common heterocyclic compound, 53297-68-0, name is 2-Chloro-4-sulfamoylaniline, molecular formula is C6H7ClN2O2S, 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 solution of the carboxylic acid and aniline shown above, in pyridine at O0C, was added POCl3 dropwise for 5 min. The reaction was complete after stirring at O0C for an additional 50 min. The reaction mixture was quenched by addition Of H2O (1 mL), then concentrated in vacuo to light brown oil which was diluted with CH2Cl2 (200 ml). The organic layer was washed with H2O (1 x 50 ml), saturated NaHCO3 solution (1 x 50 ml), then brine (1 x 50 ml). The organic solution was dried over Na2SO4 and concentrated to dryness. The resulting oil was triturated with EtOH to give light yellow solid. To the mixture was added H2O to collect more solid. The light yellow solid was collected by vacuum filtration and dried under high vacuum for 16 hrs to yield 930 mg (72%) of product. Additional product (132 mg, 10%) was recovered by extraction of the filtrate with CH2Cl2 followed by column chromatography with acetone/CH2Cl2 (20:80).
The synthetic route of 53297-68-0 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; VALEANT RESEARCH & DEVELOPMENT; WO2006/26356; (2006); A2;,
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