(2,4-dinitro-phenoxy)-acetic acid ethyl ester synthesis
- Product Name:(2,4-dinitro-phenoxy)-acetic acid ethyl ester
- CAS Number:85196-33-4
- Molecular formula:C10H10N2O7
- Molecular Weight:270.2
Yield:85196-33-4 70%
Reaction Conditions:
Stage #1: ethyl 2-hydroxyacetatewith sodium carbonate in tetrahydrofuran at 20; for 1 h;
Stage #2: 2,4-dinitrobromobenzene in tetrahydrofuran at 20; for 24 h;
Steps:
1
Specifically, ethyl glycolate (8.4 g, 80.8 mmol) was added to a solution of sodium carbonate (16.8 g, 158.4 mol) in tetrahydrofuran (50 mL).The reaction mixture was stirred at room temperature. After the reaction continued for 1 hour,The reaction material 1-bromo-2,4-dinitrobenzene (2.0 g, 4 mmol) was added.The mixture was stirred and reacted at room temperature for 24 hours.After the completion of the reaction was detected by TLC, the reaction mixture was concentrated under vacuum,Add dichloromethane and water to the concentrated reaction mixture for extraction,Wash with saturated sodium chloride solution.The dichloromethane extract was collected, dried over anhydrous sodium sulfate, and concentrated.Finally, the concentrated mixture is purified by silica gel column chromatography,The first intermediate (1.52 g, yield 70%) was obtained as a white solid.
References:
CN111978342,2020,A Location in patent:Paragraph 0064; 0081-0085
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