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ChemicalBook CAS DataBase List FLURENOL-METHYL ESTER

FLURENOL-METHYL ESTER synthesis

6synthesis methods
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Yield: 93%

Reaction Conditions:

sulfuric acid for 1 h;Heating / reflux;

Steps:

I.1.1; II.12.1
50.4 g (0. 223 mol) of 9-hydroxy-9-fluorenecarboxylic acid are dissolved in 500 ml of methanol, combined with 5 ml (0.089 mol) of CONC. sulphuric acid and refluxed for 1 hour. After cooling, 100 ml of sodium hydrogen carbonate solution (about pH 8) are added and the methanol is largely evaporated down. The mixture is extracted with dichloromethane and water, the organic phase is dried and evaporated to dryness. The product is purified by recrystallisation from ethyl acetate. Yield: 50. 0g of white crystals (= 93% of theory).

References:

BOEHRINGER INGELHEIM INTERNATIONAL GMBH;BOEHRINGER INGELHEIM PHARMA GMBH & CO. KG WO2005/13994, 2005, A1 Location in patent:Page/Page column 37; 50

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