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ChemicalBook CAS DataBase List 2-AMINOPHENOL HYDROCHLORIDE

2-AMINOPHENOL HYDROCHLORIDE synthesis

4synthesis methods
-

Yield:51-19-4 90%

Reaction Conditions:

with hydrogenchloride in methanol for 15 h;Inert atmosphere;

Steps:

1.1 1-1:
Preparation of hydrazine salt
1-1:
Preparation of hydrazine salt
In a 1-liter 4-neck flask, 50g (0.46 mol) of the compound of Chemical Formula 6 (2-amino phenol) was completely dissolved in 500 ml (11.5 mol) of methanol (MeOH) with vigorous stirring. To a separate 500 ml flask equipped with a dropping funnel was placed 134 g (2.3 mol) of NaCl, and the dropping funnel was filled with 113 g (1.15 mol) of conc. sulfuric acid (H2SO4) . As H2SO4 was slowly added from the funnel, HCl gas was generated. The HCl gas was introduced into the 1-L flask while stirring. After completion of gas generation, the separate 500 ml flask was removed, and stirring was continued for 15 hrs in the HCl gas-injected reactor. Then, the reactor was purged with N2, followed by vacuum concentration to evaporate about 3/4 (400 ml) of the solvent. Ethyl acetate (EA) (1 L) was added to form a precipitate while stirring for 30 min or longer. The precipitate was an HCl salt of 2-aminophenol, and washed with 200 ml of a mixture of ethyl acetate (EA) and hexane (3:7), and dried in a vacuum to give 60 g of the compound of Chemical Formula 7 (yield: 90%).

References:

Korea Institute of Ocean Science and Technology;YIM, Joung Han;KIM, Il Chan;KIM, Dockyu;HAN, Se Jong;LEE, Hyoung Seok;BHATTARAI, Hari Datta;KIM, Tai Kyoung;KIM, Keun Sik EP2816028, 2014, A1 Location in patent:Paragraph 0032; 0033; 0034; 0035; 0036; 0037

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