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ChemicalBook CAS DataBase List 9-Hydroxyxanthene
90-46-0

9-Hydroxyxanthene synthesis

12synthesis methods
synthesis of xanthydrol: The amalgam sodium in dry toluene was warmed to 50°C, the xanthone-ethanol suspension was added, and the temperature was rapidly raised to 60-70°C with vigorous stirring. After the reaction is completed, the mercury is separated. The reaction solution was filtered, the filtrate was poured into the stirred blue distilled water, the 9-hydroxyxanthene was filtered out, washed with water, and dried to obtain the finished product with a yield of 91-95%.
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Yield:90-46-0 94%

Reaction Conditions:

with ethanol;sodium hydroxide;zinc at 20; for 4 h;Reflux;Concentration;

Steps:

2 Tons alcohol synthesis

Tonnes (294.3 g, 1.5 mol, 1.0 eq) and ethanol (1800 mL) were added to a 3 L four-necked flask and stirred at room temperatureAfter dissolving, sodium hydroxide solid (480 g, 12.0 mol, 8.0 eq) was added, and then the temperature was raised to 50 ° C. The reduced Zn(195g, 3.0mol, 2.0eq). After the addition was completed, the mixture was heated to reflux for 4h. The disappearance of the starting material by TLC (VPE / EA = 5: 1)After completion of the reaction, hot filtered to remove the solid, and then concentrated under reduced pressure to remove most of the ethanol, the residue was added 6mol / L dilute hydrochloric acidAdjust the pH = 7, the solid precipitated, filtered, vacuum dried at 50 ° C to give 279g tyl alcohol, the yield was 94%

References:

CN107353275,2017,A Location in patent:Paragraph 0035; 0036; 0037; 0044; 0045; 0046

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