3-Chloro-5-chlorosulfonyl-benzoic acid synthesis
- Product Name:3-Chloro-5-chlorosulfonyl-benzoic acid
- CAS Number:53553-11-0
- Molecular formula:C7H4Cl2O4S
- Molecular Weight:255.08
535-80-8
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Yield:53553-11-0 41%
Reaction Conditions:
with chlorosulfonic acid for 12 h;Heating;Inert atmosphere;
Steps:
132 Synthesis of compound 132.1.
Into a 50-mL round-bottom flask purged and maintained with an inert atmosphere of nitrogen, was placed 3-chlorobenzoic acid (3 g, 19.16 mmol, 1 equiv), HSO3Cl (5 mL). The resulting solution was stirred for 12 hr at 130oC in an oil bath. The reaction was then quenched by the addition of 20 mL of water/ice. The resulting solution was extracted with 3x20 ml of ethyl acetate. The resulting mixture was washed with 1 x20 ml of brine. The mixture was dried over anhydrous sodium sulfate and concentrated. The resulting mixture was concentrated. This resulted in 2 g (yield = 41%) of 132.1 as a yellow solid. (ES, m/z): [M-H]- 252.9.
References:
WO2020/97408,2020,A1 Location in patent:Paragraph 00466
855471-53-3
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53553-11-0
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