4-AcetaMido-3-broMobenzoic acid synthesis
- Product Name:4-AcetaMido-3-broMobenzoic acid
- CAS Number:74103-28-9
- Molecular formula:C9H8BrNO3
- Molecular Weight:258.07
103-89-9
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Yield:74103-28-9 95%
Reaction Conditions:
with (trifluoromethyl)benzene;bromine in lithium hydroxide monohydrate at 20; for 24 h;Irradiation;
Steps:
General procedure of oxidation of toluenes into carboxylic acids
General procedure: A 100-mL-pyrex flask was charged with 1 (5.0 mmol) and Br2 (840 mg, 10.5 mmol) in BTF (30 mL) andwater (6 mL). The attached reflux condenser was open air, and the flask was irradiated with a 13-Wwhite-fluorescent lamp, 40-W-blue LED (454 nm), or 10-W-UV LED (385 nm) at intervals of 5 cm withvigorous stirring for 24 h. Saturated aqueous NaHCO3 and EtOAc were added to the reaction mixture.The alkaline aqueous layer was separated and acidified with diluted HCl. The solution was successivelyextracted using EtOAc and washed with water and brine. A concentrated product 2 was produced afterdrying over anhydrous Na2SO4. The samples were sufficiently pure, without requiring furtherpurification.
References:
Kirihara, Masayuki;Sakamoto, Yugo;Yamahara, Sho;Kitajima, Atsuhito;Kugisaki, Naoki;Kimura, Yoshikazu [Synlett,2022,vol. 33,# 16,p. 1670 - 1674] Location in patent:supporting information
614-83-5
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556-08-1
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103-88-8
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23373-04-8
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101209-08-9
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2719-21-3
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