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ChemicalBook CAS DataBase List 4-Aminobenzoic acid
150-13-0

4-Aminobenzoic acid synthesis

13synthesis methods
4-Aminobenzoic acid synthesis method: add 38.0g of p-nitrobenzoic acid, 200mL of water, 20mL of tetrahydrofuran, 0.4g of sodium dodecyl sulfonate and 1.9g of Raney nickel to the autoclave, nitrogen replacement Three times, fill with hydrogen, adjust the pressure to 0.9±0.1MPa, adjust the temperature to 100±2°C, and keep the reaction under pressure for 4h to complete. After the reaction, the catalyst was recovered by filtration, left to stand for stratification, the water layer was directly applied mechanically, the tetrahydrofuran layer was distilled and recovered and applied mechanically, then 1.5 g of activated carbon was added to the 4-aminobenzoic acid mother liquor, and under nitrogen protection, heating and refluxing for decolorization for 20min, Filtration, cooling and crystallization of mother liquor, filtration, drying under vacuum at 80-85 °C to obtain 30.3 g of 4-aminobenzoic acid with a yield of 97.2%, a melting point of 187.1-187.6 °C, and a content of 100.2% (permanent stop titration method) .
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Yield:2835-68-9 94% ，150-13-0 6%

Reaction Conditions:

with water at 140; for 6 h;Sealed tube;

Steps:

2.3 General Reaction Procedure

General procedure: In a typical reaction procedure 1 mmol benzonitrile and3 ml of H2O was taken in a sealed tube. About 80 mg ofcatalyst was added to this reaction mixture and stirred at140 °C on a oil bath for stipulated reaction time. Theprogress of the reaction was monitored by using thin layerchromatography. The products were identified by GC-MS(SHIMADZU-2010) analysis by separating the products ona DB-5 column.

References:

Srinivasa Rao;Srivani;Dhana Lakshmi;Lingaiah [Catalysis Letters,2016,vol. 146,# 10,p. 2025 - 2031]

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