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ChemicalBook CAS DataBase List 6-Hydroxy-1-naphthoic acid

6-Hydroxy-1-naphthoic acid synthesis

8synthesis methods
-

Yield:2437-17-4 19.7 g

Reaction Conditions:

with aluminum (III) chloride in N,N-dimethyl-formamide at 135; for 6 h;Solvent;

Steps:

3 Example 3

In a 250ml four-necked bottle, add 20g of furoic acid, 23.2g of anisole, 100ml chlorobenzene, stirred and mixed; oil bath heated to internal temperature 35 ~ 40 ° C, slowly added 55.9g anhydrous aluminum trichloride; after the completion of the feed, stirring at 75-80 ° C for about 24 hours; cooling, concentrated distillation under reduced pressure Chlorobenzene After the distillation was completed, the temperature was lowered to room temperature, 60 ml of N,N-dimethylformamide was added to the reaction flask, and the mixture was stirred and mixed. At room temperature, 32.1 g of anhydrous aluminum trichloride was slowly and separately added; after the completion of the feeding, the oil bath was heated to The internal temperature is 135 ° C, and the reaction is kept for 6 hours; The water is cooled to room temperature; the reaction solution is slowly added to dilute hydrochloric acid solution for hydrolysis; extracted with ethyl acetate several times, and the ethyl acetate extract is combined, washed with water, and Ph is weakly acidic; The organic layer was concentrated under reduced pressure to recover ethyl acetate; The residue is decolorized and recrystallized with dilute alcohol water. Yielding 19.7 g of 6-hydroxy-1-naphthoic acid as a gray to pale yellow powder. Yield: 58.7%, melting point: 205.5 to 208.6 ° C, purity: 98.5%.

References:

CN108863775,2018,A Location in patent:Paragraph 0035; 0037; 0038-0039; 0041; 0043; 0045; 0047

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