* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.
With aluminum (III) chloride In dichloromethane at 33 - 37℃; for 6 h;
15.8 g of 1-methoxynaphthalene and 10.0 g of succinic anhydride were dissolved in 120 mL of dichloromethane,Stir,Cooling to 1 ~ 3 ° C,Divided into three batches of anhydrous aluminum trichloride 15.0 grams,The addition process takes about 20 minutes,The solution was then heated to 35 ± 2 ° C,Insulation reaction 6 hours (5.5 ~ 6.5 hours range),After the reaction is complete,The reaction solution was poured into an ice-water mixture (200 g of ice and 300 g of water) for 30 minutes,Standing, analysiscrystal,Filter,The filtrate was heated and distilled to recover dichloromethane,The cake is the crude of the ketone ketone;And then the crude ketoprofen water as a solvent by 2-3 times recrystallization,Activated carbon decolorization,Demon ketone boutique.The mass of the present product of the chamballone was 22.3 g,Melting point of 176 ~ 179 ° C,The yield was 86.4percent.
Reference：
[1] Patent: CN104370734, 2016, B, . Location in patent: Paragraph 0016-0018
[2] Helvetica Chimica Acta, 1932, vol. 15, p. 907,914
[3] Journal of the University of Bombay, Science: Physical Sciences, Mathematics, Biological Sciences and Medicine, 1936, vol. 5/2, p. 73,75
[4] Journal of the American Chemical Society, 1940, vol. 62, p. 2750,2752
[5] Journal of the American Chemical Society, 1951, vol. 73, p. 897,899
[6] Journal of the American Chemical Society, 1951, vol. 73, p. 326,327
[7] Kogyo Kagaku Zasshi, 1953, vol. 56, p. 887,889[8] Chem.Abstr., 1955, p. 6904
[9] Journal of the American Chemical Society, 1936, vol. 58, p. 2314,2316
[10] Bulletin de la Societe Chimique de France, 1968, p. 627 - 631
[11] Fortschr. Teerfarbenfabr. Verw. Industriezweige, vol. 14, p. 285
2
[ 108-30-5 ]
[ 75-15-0 ]
[ 7446-70-0 ]
[ 2216-69-5 ]
[ 3562-99-0 ]
Reference：
[1] Journal of the American Chemical Society, 1936, vol. 58, p. 2314,2316
[2] Helvetica Chimica Acta, 1932, vol. 15, p. 907,914
[3] Journal of the University of Bombay, Science: Physical Sciences, Mathematics, Biological Sciences and Medicine, 1936, vol. 5/2, p. 73,75
3
[ 108-30-5 ]
[ 7446-70-0 ]
[ 630-20-6 ]
[ 2216-69-5 ]
[ 3562-99-0 ]
Reference：
[1] Journal of the American Chemical Society, 1936, vol. 58, p. 2314,2316
[2] Helvetica Chimica Acta, 1932, vol. 15, p. 907,914
[3] Journal of the University of Bombay, Science: Physical Sciences, Mathematics, Biological Sciences and Medicine, 1936, vol. 5/2, p. 73,75
4
[ 108-30-5 ]
[ 7446-70-0 ]
[ 98-95-3 ]
[ 2216-69-5 ]
[ 3562-99-0 ]
Reference：
[1] Journal of the American Chemical Society, 1936, vol. 58, p. 2314,2316
[2] Helvetica Chimica Acta, 1932, vol. 15, p. 907,914
[3] Journal of the University of Bombay, Science: Physical Sciences, Mathematics, Biological Sciences and Medicine, 1936, vol. 5/2, p. 73,75
With trifluoroacetic acid; trifluoroacetic anhydride; at 20℃; for 12.0h;
General procedure: A mixtureof 1 (12 mmol), phenylacetic acids 2a-2s (8 mmol), andtrifluoroacetic anhydride (16 mmol) in trifluoroacetic acid(5 mL) was stirred at room temperature for overnight. Afterthe completion of the reaction, the content was poured intowater (100 mL) and extracted with ethyl acetate (100 mL × 3).The combined organic extracts were dried over Na2SO4, filtered,and concentrated. The residue was purified by chromatographyto give the product 3a-3s, which containing someimpurities. These compounds were used in the next step without further purification.
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