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CAS No. : | 117-78-2 | MDL No. : | MFCD00001231 |
Formula : | C15H8O4 | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | ASDLSKCKYGVMAI-UHFFFAOYSA-N |
M.W : | 252.22 | Pubchem ID : | 67030 |
Synonyms : |
|
Chemical Name : | 9,10-Dioxo-9,10-dihydroanthracene-2-carboxylic acid |
Signal Word: | Warning | Class: | N/A |
Precautionary Statements: | P261-P305+P351+P338 | UN#: | N/A |
Hazard Statements: | H302-H315-H319-H335 | Packing Group: | N/A |
GHS Pictogram: |
* 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.
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
85% | With chromium(VI) oxide; acetic acid; at 85℃; for 16h; | 2-Methylanthraquinone (1) (1 g, 4.5 mmol) and acetic acid (50 mL) were added to a double-necked flask fittedwith a condenser. A mechanical stirrer and a thermocouple were also placed into the flask. The reactionmixture was warmed gently with stirring to dissolve 2-methylanthraquinone. Then anhydrous CrO3 (5.4 g,54 mmol) was added slowly with vigorous stirring. The solution mixture was heated to 85 C and kept atthat temperature overnight (16 h) with stirring. Then the completed reaction mixture was cooled at roomtemperature and diluted with 150 mL of distilled water. The resulting precipitate was filtered and washedwith water until the blue color of chromium salts disappeared. The obtained solid was recrystallized in aceticacid to yield anthraquinone-2-carboxylic acid (2) as white crystalline solid. Yield: 85percent. 1 H NMR (400 MHz,DMSO-d6) 13.73 (s, 1H), 8.64 (d, J = 1.7 Hz, 1H), 8.38 (dd, J = 8.0, 1.6 Hz, 1H), 8.28 (dd, J = 8.0, 1.9Hz, 1H), 8.21 (dd, J = 5.1, 2.2 Hz, 2H), 8.01?7.90 (m, 2H). 13 C NMR (100 MHz, d6 -DMSO) 181.9, 181.8,165.9, 135.6, 135.5, 134.7, 134.7, 134.4, 133.1, 133.0 (2C), 127.3, 127.2, 126.8 (2C). |
42.9% | With chromium(VI) oxide; acetic acid; at 80 - 120℃; for 1h; | To a 500 mL reaction flask was added 2-methyl-9,10-anthraquinone (8.9 g, 40 mmol) And glacial acetic acid (180 mL, 20 mL / g), stirred at 80 ° C, Silica oxide (40 g, 0.4 mol) was slowly added in portions, After the temperature is stable, the temperature is raised to 120 ° C. After cooling, the mixture was washed with water to obtain 4.32 g of a pale yellow cotton solid in a yield of 42.9percent. |
With ammonium hydroxide; sodium dichromate; In sulfuric acid; water; | Reference Preparation 6 -Anthraquinone-2-carboxylic acid. 2-Methylanthraquinone (3 g.) was dissolved in sulphuric acid (15 ml) and the solution cooled and diluted with water (15 ml) The mixture was then cooled and stirred vigorously during the portionwise addition of powdered sodium dichromate (9 g.) and finally heated on the steam-bath for 3 hours, cooled and treated with water (100 ml.). The precipitated solid was filtered, washed well with water and treated with hot dilute aqueous ammonia (60 ml. water and 2 ml. of 0.880 ammonia). The solution was filtered hot and acidified with hydrochloric acid; the pale yellow precipitate was filtered, washed with water and dried to give anthraquinone-2-carboxylic acid, m.p. 291°-292° unchanged by recrystallisation from dimethylformamide. |
With ammonium hydroxide; sodium dichromate; In sulfuric acid; water; | REFERENCE PREPARATION 6 Anthraquinone-2-carboxylic acid 2-Methylanthraquinone (3 g.) was dissolved in sulphuric acid (15 ml) and the solution cooled and diluted with water (15 ml). The mixture was then cooled and stirred vigorously during the portionwise addition of powered sodium dichromate (9 g.) and finally heated on the steam-bath for 3 hours, cooled and treated with water (100 ml.). The precipitated solid was filtered washed well with water and treated with hot dilute aqueous ammonia (60 ml. water and 2 ml. of 0.880 ammonia). The solution was filtered hot and acidified with hydrochloric acid; the pale yellow precipitate was filtered, washed with water and dried to give anthraquinone-2-carboxylic acid, m.p. 291°-292° unchanged by recrystallisation from dimethylformamide. |
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