Ethyl L-valinate hydrochloride synthesis
- Product Name:Ethyl L-valinate hydrochloride
- CAS Number:17609-47-1
- Molecular formula:C7H16ClNO2
- Molecular Weight:181.66
64-17-5
72-18-4
17609-47-1
The general procedure for the synthesis of L-valine ethyl ester hydrochloride from ethanol and L-valine is as follows: 5 kg (42.7 mol) of L-valine and 4 kg of anhydrous ethanol were added to a 50-liter glass reactor and stirred until complete dissolution. After cooling the reaction mixture to 0-10°C, 8.8 liters of thionyl chloride were added slowly and dropwise. After the dropwise addition was completed, the reaction mixture was gradually heated to reflux and the reaction was maintained for 18 hours. Upon completion of the reaction, the reaction solution was concentrated to dryness. Subsequently, 15 liters of isopropyl acetate was added to the dried residue at 15 to 20°C and stirred for 1 hour. Finally, the product was collected by diafiltration to give 6.1 kg of off-white solid, Intermediate 1 (where R1 is ethyl).
Yield:17609-47-1 97.23%
Reaction Conditions:
with hydrogenchloride in water at 20; for 12 h;
Steps:
2 Example 2
At room temperature, dry hydrogen chloride gas was introduced into a 500 ml four-necked flask of 300 ml ofethanol and 50 g of valine until the hydrochloric acid reached saturation, and the tail gas was absorbed in anethanol solution. The reaction was started for 12 hours until the proline content was reached. Less than 1% is theend of the reaction, the ethanol is evaporated under reduced pressure, the residue is added with ethyl acetate, themixture is cooled to 0 ° C, stirred for 1 hour, filtered and dried to give a valine alkyl ester, the yield is 97.23%,the product purity is 99.30. %, optical purity 99.32%.
References:
Jiangsu Xin Rui Pharmaceutical Co., Ltd.;Cao Enqing;Wang Qiuhua;Wang Xiuyun;Wang Li;Zhao Xuesong CN108892622, 2018, A Location in patent:Paragraph 0017; 0018
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