pyridine-3-sulfonyl chloride synthesis
- Product Name:pyridine-3-sulfonyl chloride
- CAS Number:16133-25-8
- Molecular formula:C5H4ClNO2S
- Molecular Weight:177.61
636-73-7
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16133-25-8
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Yield:16133-25-8 94%
Reaction Conditions:
with phosphorus pentachloride;trichlorophosphate for 3 h;Heating / reflux;
Steps:
B.1.1
A mixture of pyridine-3-sulfonic acid (10.3 g, 64.8 mmol), phosphorus pentachloride (20.82 g, 100 mmol) and phosphorus oxychloride (10 mL, 109 mmol) was heated to reflux for 3 h (according to J. Org. Chem. 1989, 54(2), 389.). Evaporated to dryness to give a yellow solid, dissolved in ice water and methyl-tert-butyl ether, added cautiously sat. NaHCO3-sol. until neutralized, saturated with solid NaCl, separated phases, dried organic layer over Na2SO4. Removal of the solvent in vacuum to give the title compound as an orange liquid (10.85 g, 94%). MS (ISP) 178.1 [(M+H)+] and 180.0 [(M+2+H)+].
References:
US2006/217387,2006,A1 Location in patent:Page/Page column 25
462-08-8
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16133-25-8
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42899-76-3
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16133-25-8
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626-55-1
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16133-25-8
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16133-26-9
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16133-25-8
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