Hydrochloric Acid → HCID 57167397, compound

Participants

Reaction Conditions

Reaction Steps

To a solution of hydroxylamine hydrochloride (11.6 g; 0.17 mol) in methanol (80 mL) was added at 40° C. and with stirring a solution of sodium methoxide in methanol (80 mL) prepared from 7.7 g (0.33 mol) of sodium. To this solution was added at 0° C. a solution of crude (V) (31.6 g; ca. 0.11 mol) in methanol (40 mL). This mixture was left at 25° C. with stirring for 24 h, and after cooling to 0° C. and with continued stirring, pH of the solution was adjusted to ca. 3 by addition of a solution of hydrogen chloride in ethyl acetate (2.5 M). The filtered and evaporated reaction mixture was extracted with ethyl acetate, and after filtration and addition of light petroleum (50 mL) compound (IV) crystallized. The yield of (IV) was 12.0 g (39%), M.p. 152.0-154.0° C. Anal. C11H18N2O6.

Provenance & Evidence