DL-Ethyl 2-bromobutyrate synthesis
- Product Name:DL-Ethyl 2-bromobutyrate
- CAS Number:533-68-6
- Molecular formula:C6H11BrO2
- Molecular Weight:195.05
Yield:533-68-6 98.5%
Reaction Conditions:
with potassium hydrogensulfate at 70 - 90; for 2 h;Large scale;Reagent/catalyst;
Steps:
1-2
Add 1000 kg of 2-bromobutyric acid to a 2000 L esterification reactor.800 kg of ethanol, 100 kg of anhydrous potassium bisulfate was added.When the stirring is started, the temperature is raised. When the temperature rises to about 70 ° C, the heating is stopped, and the reflux is slowly generated.As the temperature increases, the reflux gradually increases, refluxing for 2 hours, when the temperature rises to 85-90 ° C, after the GC detection of the raw material 2-bromobutyric acid reaction is completed, the ethanol is slowly distilled off.After distilling off the ethanol, the mixture is repeatedly filtered and dried under anhydrous potassium hydrogen sulfate, and the ethanol is dried and then returned to the next batch.The filtered ethyl 2-bromobutyrate was neutralized with a soda ash and transferred to a rectification distillation.The jet water pump and the Roots pump are used to distill the product, and the fraction is collected to obtain a brominated fatty acid ester.1150kg, content 99.08%, yield 98.5%.
References:
Dafeng Jingyuan Fine Chemical Co., Ltd.;Tang Jianye;Jiang Bufang CN109503354, 2019, A Location in patent:Paragraph 0020; 0022-0023; 0025
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