Ethyl (3E)-3-(2-phenylhydrazin-1-ylidene)butanoate synthesis
- Product Name:Ethyl (3E)-3-(2-phenylhydrazin-1-ylidene)butanoate
- CAS Number:6078-46-2
- Molecular formula:C12H16N2O2
- Molecular Weight:220.27
Yield:6078-46-2 90.4%
Reaction Conditions:
in ethanol at -5 - 0; for 1 h;Solvent;
Steps:
3.1
(1) 108g of phenylhydrazine addedInto 864mL ethanol,Add 136.5g ethyl acetoacetate under temperature control -50,React at -5°C for 1 hour,After the reaction, take out half of the reaction solution and addThe mass fraction is 100 mL of 20% sodium bicarbonate solution to quench the reaction,Add dichloromethane to extract,Concentrate under reduced pressure at 35°C to obtain an oily substance,Column chromatography purification, drying,Obtained 99.76g of transition state impurities,The yield was 90.4%.
References:
CN113072502,2021,A Location in patent:Paragraph 0023; 0038; 0042; 0046; 0047; 0054
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