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Piperidine, 4-bromo-1-[(4-methylphenyl)sulfonyl]- synthesis

7synthesis methods
-

Yield:347885-68-1 97%

Reaction Conditions:

with pyridine at 20 - 30; for 24 h;Inert atmosphere;

Steps:

1 Preparation Example 1

Under the protection of argon, add 4-bromopiperidine hydrogen bromide (2.45g, 10mmol) to the reaction flask equipped with a stir bar, pyridine (30mL) is fully dissolved, and p-toluenesulfonyl chloride (2.86 g, 15mmol), react at room temperature for 24h. Add deionized water to the system to quench the reaction, spin off a large amount of pyridine, 1M hydrochloric acid/dichloromethane to extract the organic phase, dry with anhydrous sodium sulfate, concentrate, silica gel column chromatography, eluent is petroleum ether: ethyl acetate: Dichloromethane=10:1:1 to 10:1:2, the product is a white solid 3.10g, the yield is 97%, and the 1H NMR purity is greater than 98%.

References:

CN112142544,2020,A Location in patent:Paragraph 0106-0109