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ChemicalBook CAS DataBase List Oxazosulfyl
1616678-32-0

Oxazosulfyl synthesis

9synthesis methods
2-Pyridinecarboxamide, 3-(ethylsulfonyl)-N-[2-hydroxy-5-[(trifluoromethyl)sulfonyl]phenyl]-

1616679-29-8
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Oxazosulfyl

1616678-32-0
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Yield:1616678-32-0 99%

Reaction Conditions:

with acetic anhydride;toluene-4-sulfonic acid in water;1,3,5-trimethyl-benzene at 165; for 11 h;Inert atmosphere;Dean-Stark;Reagent/catalyst;Solvent;Temperature;

Steps:

1; 2; 3; 4; 1 Example 4

Under the nitrogen atmosphere, a mixture of 38.2 g of paratoluenesulfonic acid monohydrate and 38.4 g of mesitylene was refluxed and dehydrated for 2 hours and 40 minutes using a Dean-Stark apparatus. To a mixture of 83.7 g of a compound (2) and 201 g of mesitylene was added the previously obtained mixture of paratoluenesulfonic acid and mesitylene. The resulting mixture was heated to 165° C., and 16.77 g of acetic anhydride was added dropwise over 11 hours, while distilling off water, acetic acid, and mesitylene. An amount of the distilled off liquid at that time was 146 g, and that of mesitylene added dropwise was 147 g. The reaction rate of the resulting mixture was determined using high performance liquid chromatography, and found to be99%.

References:

US2019/2451,2019,A1 Location in patent:Paragraph 0017; 0019; 0020; 0021; 0022