Ethyl 2-(4-hydroxyphenyl)-2-oxoacetate synthesis
- Product Name:Ethyl 2-(4-hydroxyphenyl)-2-oxoacetate
- CAS Number:70080-54-5
- Molecular formula:C10H10O4
- Molecular Weight:194.18
Yield:70080-54-5 60%
Reaction Conditions:
with aluminum (III) chloride in dichloromethane at 0 - 20; for 6 h;
Steps:
1 Preparation of ethyl (4-hydroxyphenyl)-2-oxalate (Intermediate II-A)
Dissolve phenol (2.00g, 21.25mmol) in dichloromethane, stir under ice bath,Slowly add aluminum trichloride (5.67 g, 42.50 mmol).Add oxalyl chloride (3.48g, 25.50mmol) slowly to the above solution,After the addition, the reaction solution gradually rose from zero degrees Celsius to room temperature, and reacted at room temperature for 6 hours.After the reaction is over, the reaction solution is slowly poured into ice water with constant stirring.Extract with dichloromethane, wash with water and saturated sodium chloride aqueous solution, and dry the organic phase with anhydrous sodium sulfate.The organic solvent was removed by rotary evaporation, and the intermediate was separated by silica gel column chromatography.(4-Hydroxyphenyl)-2-oxalic acid ethyl ester (Intermediate -A),2.5g, white solid, yield 60%.
References:
CN111825605,2020,A Location in patent:Paragraph 0132-0134
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