2-chloro-5-(methylsulphamoyl)benzoic acid synthesis
- Product Name:2-chloro-5-(methylsulphamoyl)benzoic acid
- CAS Number:68901-09-7
- Molecular formula:C8H8ClNO4S
- Molecular Weight:249.67
Yield:68901-09-7 96%
Reaction Conditions:
in 1,4-dioxane;water at 20; for 2 h;
Steps:
25.a
To 41.9 mmol 2-chloro-5-(fluorosulfonyl)sulfanyl-benzoic acid in 100 ml dioxane was added dropwise 420 mmol methylamine solution (41% aqueous) and the mixture was stirred at RT for 2 h. An excess of 2 M aqueous hydrochloric acid was then added to the reaction mixture and the resulting mixture was then concentrated in vacuo. The residue was treated with water and extracted 3 times with ethyl acetate. The combined organic phases were dried over sodium sulfate. Evaporation under reduced pressure yielded the title compound as a white crystalline solid (yield 96%). MS (m/e): 248.1 ([M-H]-, 100%).
References:
US2006/149062,2006,A1 Location in patent:Page/Page column 16
