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ChemicalBook CAS DataBase List 2-Aminoethylmethylsulfone hydrochloride
104458-24-4

2-Aminoethylmethylsulfone hydrochloride synthesis

3synthesis methods
Carbamic acid, N-[2-(methylsulfonyl)ethyl]-, 1,1-dimethylethyl ester

154095-06-4

2-Aminoethylmethylsulfone hydrochloride

104458-24-4

Under the condition of cooling in an ice bath, tert-butyl 2-(methylsulfonyl)ethylcarbamate (1.5 g) was dissolved in ethyl acetate (10 mL), and ethyl acetate solution of 4N hydrochloric acid (3 mL) was added slowly and dropwise with stirring. After the reaction mixture was stirred at room temperature overnight, the precipitated solid was collected by filtration and washed with ethyl acetate to give 2-(methylsulfonyl)ethylamine hydrochloride (1.04 g, 97% yield). The product was recrystallized from ethanol to give colorless prismatic crystals with a melting point of 169-170 °C.

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Yield:104458-24-4 94.8%

Reaction Conditions:

with hydrogenchloride;dihydrogen peroxide in water; pH=3 - 4 at 25 - 30;Solvent;

Steps:

1.2 Synthesis of 2-(methylsulfonyl)ethylamine hydrochloride
2000ml three bottles,Was added 2- (methylthio) ethylamine (91 g, 1 mol) and 500 ml of water,With 37% concentrated hydrochloric acid to adjust the pH to 3 ~ 4,Keep the temperature 25 ~ 30 ,Dropping 30% hydrogen peroxide solution (240g, 2.1mol), 1 ~ 1.5h drop finished,The reaction was carried out at 25 to 30 ° C for 10 hours,The solvent was distilled off under reduced pressure,The residue was added to 500 ml of ethanol,Precipitation of white solid,filter,Ethanol wash,60 under reduced pressure to dry 151.2g,Is 2- (methylsulfonyl) ethylamine hydrochloride,Yield 94.8%The purity of the product is 99.8% (GC method).

References:

Shandong Boyuan Pharmaceutical Co., Ltd.;Li Taitong;Wang Qun CN107056661, 2017, A Location in patent:Paragraph 0011; 0029; 0032; 0033; 0035-0037

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