ChemicalBook CAS DataBase List p-Aminobenzoesure-2-ethylhexylester

p-Aminobenzoesure-2-ethylhexylester synthesis

4synthesis methods

Product Name:p-Aminobenzoesure-2-ethylhexylester
CAS Number:26218-04-2
Molecular formula:C15H23NO2
Molecular Weight:249.35

4-NITRO BENZOIC ACID 2-ETHYL-HEXYL ESTER

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26218-04-2
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Yield:26218-04-2 99.2%

Reaction Conditions:

with palladium on activated charcoal;hydrogen in water at 50 - 60; under 750.075 - 3000.3 Torr;Sealed tube;

Steps:

1 Hydrogenation:
Put 619.8g of isooctyl p-nitrobenzoate in isooctyl alcohol into a dry and clean 2L hydrogenation kettle,2.1gPd/C (~5%, water content~60%), and 223.1g isooctyl alcohol;At the end of feeding, seal the hydrogenation kettle, replace it with nitrogen 3 times, and replace it 3 times with hydrogen; open the hydrogenation kettle and stir, set the hydrogen pressure in the kettle to 0.1-0.4Mpa, and the temperature of the kettle to 50-60°C. The hydrogenation reaction was started. During the reaction, the temperature of the kettle was maintained at 50-60°C. When the reaction did not absorb hydrogen any more, samples were taken and sent to GC for detection. When the isooctyl p-nitrobenzoate <0.1%, the reaction was stopped. Close the hydrogen main valve, lower the temperature of the kettle to 30-40°C, open the drain valve of the hydrogenation kettle, discharge the pressure in the kettle to 0.02Mpa, and replace the hydrogen in the kettle with nitrogen 3 times. The discharge port of the hydrogenation kettle was opened, and the reaction liquid was drawn out and filtered to obtain 2.3 g of catalyst and 847.3 g of filtrate. The catalyst was used in batch hydrogenation, and the filtrate was distilled under reduced pressure to obtain 401.3 g of isooctyl alcohol and 370.02 g of hydrogenation product isooctyl p-aminobenzoate. The GC purity was 99.56% and the yield was 99.2% (calculated as p-nitrobenzoic acid).

References:

CN112321522, 2021, A Location in patent:Paragraph 0071; 0095; 0097

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