35623-11-1, name is 3-[(Methylamino)sulphonyl]benzoic Acid, belongs to amides-buliding-blocks compound, is considered to be a conventional heterocyclic compound, which is widely used in drug synthesis. The chemical synthesis route is as follows. Application In Synthesis of 3-[(Methylamino)sulphonyl]benzoic Acid
A mixture of 3-methylsulfamoyl-benzoic acid (988 mg, 4.59 mmol) and SOCl2 (5 ml) was stirred at 70 C for 10 h. The mixture was concentrated under reduced pressure and azeotroped with toluene to give the crude carboxylic acid chloride. n-BuLi (5.83 ml, 15.2 mmol, 2.6 M in hexane) was added to a solution of 1,1,1,3,3,3- hexamethyldisilazane (3.2 ml, 15.2 mmol) in THF (15 ml) at -78 C. After stirring for 1 h at -78 C, ?- butyrolactone (395 mg, 4.59 mmol) in THF (5 ml) was added. After stirring for 15 min at -78 C, crude acid chloride in THF (15 ml) was added to the reaction mixture. The mixture was allowed to slowly warm to room temperature and stirring was continued for 1 h. The mixture was acidified with 5 M HCl aq. and extracted with diethyl ether twice. The combined organic extract was washed with brine, dried over Na2SO4, filtered and concentrated under reduced pressure. The residue was purified by flash column chromatography (n-hexane/EtOAc) to afford the titled compound (1.43 g, quant.) as colorless oil.
The synthetic route of 35623-11-1 has been constantly updated, and we look forward to future research findings.
Reference:
Article; Kawada, Hatsuo; Ebiike, Hirosato; Tsukazaki, Masao; Nakamura, Mitsuaki; Morikami, Kenji; Yoshinari, Kiyoshi; Yoshida, Miyuki; Ogawa, Kotaro; Shimma, Nobuo; Tsukuda, Takuo; Ohwada, Jun; Bioorganic and Medicinal Chemistry Letters; vol. 23; 3; (2013); p. 673 – 678;,
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