Methyl 3-aminopropionate hydrochloride synthesis
- Product Name:Methyl 3-aminopropionate hydrochloride
- CAS Number:3196-73-4
- Molecular formula:C4H10ClNO2
- Molecular Weight:139.58
67-56-1
107-95-9
3196-73-4
Under ice bath conditions, 60 mL of methanol was added to a 100 mL round-bottom flask, followed by the slow dropwise addition of 4 mL of sulfoxide chloride (SOCl2) through a constant-pressure dropping funnel (with a desiccant tube at the top), and the resulting off-gas was absorbed with NaOH solution. After stirring the reaction mixture for 1 h, 8 mmol of β-alanine was added and stirring was continued for 30 min at room temperature. Subsequently, the reaction system was warmed up to 66 °C and refluxed for 6 hours. The reaction process was monitored by thin-layer chromatography (TLC) using a 2% ethanol solution of ninhydrin as a color developer until the raw material spot disappeared. Upon completion of the reaction, the solvent was removed by distillation to afford methyl 3-aminopropionate hydrochloride in 100% yield.
Yield:3196-73-4 100%
Reaction Conditions:
Stage #1:methanol with thionyl chloride for 1 h;Cooling with ice;
Stage #2:3-amino propanoic acid at 20 - 66; for 6.5 h;
Steps:
15.2 (2)Preparation of β-alanine methyl ester methyl ester hydrochloride
Under ice bath, 100 ml round-bottom flask was added with 60 ml of methanol, and then slowly added with 4 ml of SOCl2 through constant pressure dropping funnel (with a drying tube on the top), and NaOH solution was used to absorb exhaust.
After stirring for 1 h, 8 mmol of β-alanine was added and stirred at room temperature for 30 min, and then refluxed at 66° C. for 6 h.
The reaction was tracked by TLC until the raw material disappears, with a solution of 2% ninhydrin in ethanol as chromogenic reagent.
The solvent was evaporated out to obtain β-alanine methyl ester hydrochloride. Yield: 100%.
References:
Sichuan Guokang Pharmaceutical Co., Ltd;Zhang, Luyun;Yang, Fang;Shi, Wanqi;Zhang, Ping;Li, Ying;Yin, Shufan US2014/206741, 2014, A1 Location in patent:Paragraph 0016
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3196-73-4
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107-95-9
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3196-73-4
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