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ChemicalBook CAS DataBase List 2-CHLORO-6-METHOXY-3-QUINOLINECARBALDEHYDE OXIME
93299-50-4

2-CHLORO-6-METHOXY-3-QUINOLINECARBALDEHYDE OXIME synthesis

3synthesis methods
-

Yield:-

Reaction Conditions:

with hydroxylamine hydrochloride;sodium hydroxide in ethanol at 20; for 0.75 h;

Steps:

General procedure for the synthesis of 3-(2-chloroquinolin-3-yl)-5-phenylisoxazol (3a-j)

General procedure: The corresponding precursor, 2-chloroquinolin-3-carbaldehyde (2a-j) (1.0 equiv.) was added to a hydroxylamine solution (1.1 equiv.) in ethanol. Then NaOH was added (1.1 equiv.) to the reaction mixture, which was then stirred at room temperature for 45 minutes. The oxyme formation was corroborated by thin-layer chromatographic (TLC) analysis. Chloramine-T trihydrate (1.1 equiv.) was added, followed by CuSO5H2O (0.03 equiv.) and Cu (0.01 equiv.). When a change of color was observed, 10 mL of THF followed by phenylacetylene (1.1 equiv.) were added to the solution and stirred for 8 hours. Once finished, the reaction was filtered to remove copper salts, washed with water, dried with anhydrous Na2SO4 and recrystallized from ethanol. The derivatives which could not be purified using recrystallization techniques were purified using column chromatography in silica gel, using an 8:2 Hexane/EtOAc mixture as the mobile phase, except the derivative 2d, which was purified using only dichloromethane as the mobile phase.

References:

Ferna?ndez-Galleguillos, Carlos;Saavedra, Luis A.;Gutierrez, Margarita [Journal of the Brazilian Chemical Society,2014,vol. 25,# 2,p. 365 - 371]