Acetic Anhydride → HCID 178467639, compound

Participants

Reaction Conditions

Reaction Steps

3 portions of acetic acid anhydride totalling 3 ml were added at intervals of half an hour to a suspension of 0.13 g of 10-amino-3-(ethoxymethyl)-2,3-dihydro-9-hydroxy-p-dioxino [2,3-g] quinoline-8-carboxylic acid ethyl ester obtained by the method described in Example 29) in 15 ml of 96% ethanol. Before the last addition the reaction mixture was briefly heated to about 50°C, a clear solution being obtained. After the last addition the mixture was stirred for another hour and subsequently concentrated by evaporation in a vacuum. The concentrate was mixed with methylene chloride and water, after which the two layers were separated. The water layer was extracted 2 times with methylene chloride, the entire solution in methylene chloride was then washed thrice with water and subsequently dried over anhydrous sodium sulfate. Subsequently the solvent was distilled off in a vacuum. The residue having the superscribed structure was not purified any further.

Provenance & Evidence