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ChemicalBook CAS DataBase List 4-[(4-METHYLPHENYL)SULFONYL]PIPERIDINE HYDROCHLORIDE
3470-46-0

4-[(4-METHYLPHENYL)SULFONYL]PIPERIDINE HYDROCHLORIDE synthesis

6synthesis methods
Methyl 5-oxo-5,6,7,8-tetrahydronaphthalene-2-carboxylate

144464-66-4

4-[(4-METHYLPHENYL)SULFONYL]PIPERIDINE HYDROCHLORIDE

3470-46-0

Methyl 5-oxo-5,6,7,8-tetrahydronaphthalene-2-carboxylate (320 mg, 1.57 mmol) was used as a raw material and dissolved in a solvent mixture of 6 mL of methanol and 3 mL of water. Subsequently, lithium hydroxide (331 mg, 7.88 mmol) was added. The reaction mixture was stirred at room temperature for 1 h. The progress of the reaction was monitored by thin-layer chromatography (TLC), and after confirming that the reaction was complete, the pH of the reaction solution was adjusted to 5 with 1 N hydrochloric acid solution.The reaction solution was concentrated by rotary evaporation and extracted with ethyl acetate (50 mL × 2). The ethyl acetate extracts were combined and the solvent was removed by rotary evaporation to afford the white solid product 5-oxo-5,6,7,8-tetrahydronaphthalene-2-carboxylic acid (310 mg, 100% yield).

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Yield: 100%

Reaction Conditions:

with water;lithium hydroxide in methanol at 20; for 1 h;

Steps:

10 Intermediate 10-4: 5-oxo-5,6,7,8-tetrahydronaphthalene-2-carboxylic acid
Compound 10-3 (320 mg, 1.57 mmol) was dissolved in 6 mL of methanol and 3 mL of water,Lithium hydroxide (331 mg, 7.88 mmol) was added,The mixture was stirred at room temperature for 1 hour,TLC showed complete reaction,Add 1N hydrochloric acid to adjust pH = 5,Spin dry,Ethyl acetate was extracted twice (50 mL)The ethyl acetate layer was combined,Rotary evaporation to give a white solid(310 mg, 100%).

References:

Suzhou Yuanzhi Pharmaceutical Technology Co., Ltd.;Li Ben;Zhao Jian;Pei Gang;Chen Li;Jiang Tao;Zhai Peibin;Sun Li CN104844471, 2017, B Location in patent:Paragraph 0186; 0187; 0188

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