4-Ethylbenzoic acid synthesis
- Product Name:4-Ethylbenzoic acid
- CAS Number:619-64-7
- Molecular formula:C9H10O2
- Molecular Weight:150.17
1. Add ethylbenzene and trichloroacetaldehyde in the reaction kettle.
2. Add anhydrous aluminum trichloride in batches at 0 °C.
3. Stir and react at -10 ~ 0 °C for 2 hours after the addition.
4. Add dilute hydrochloric acid to the mixed solution to decompose the remaining aluminum trichloride.
5. Wash with NaHCO3 and water.
6. Distill the organic layer to recover ethylbenzene.
7. Distill to obtain p-ethylbenzene-2,2,2-trichloroethanol.
8. Dissolve the trichloroethanol in methanol.
9. Add NaOH solution and stir.
10. Add dropwise 30% hydrogen peroxide aqueous solution to the mixture.
11. Stir until the trichloroethanol disappears.
12. Acidify with HCl to obtain crystalline 4-ethylbenzoic acid.
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Yield:619-64-7 99%
Reaction Conditions:
Stage #1: 4-ethenylbenzoic acidwith palladium diacetate;4,4,5,5-tetramethyl-[1,3,2]-dioxaboralane in dichloromethane at 25; for 12 h;Schlenk technique;Inert atmosphere;
Stage #2: with hydrogenchloride in water;
Steps:
6
Replace the gas environment in the Shrek tube with a nitrogen environment, add 0.25 mmol of 4-vinylbenzoic acid, 0.0025 mmol of palladium acetate, and 0.5 mL of methylene chloride, add 0.275 mmol of pinacol borane under stirring, and react at room temperature for 12 h After the completion of the reaction, the reaction solution obtained was diluted with 10 mL of ethyl acetate, 10 mL of saturated sodium bicarbonate was added, extracted with ethyl acetate three times, the pH value of the aqueous phase was adjusted to acidic with concentrated hydrochloric acid, and then extracted with ethyl acetate, and the organic phase was taken It was concentrated under vacuum and the target product obtained in> 99% yield was a white solid.
References:
CN111099986,2020,A Location in patent:Paragraph 0034; 0065-0068
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