Benzenesulfonic acid, 4-methyl-, compd. with pyridine (1:1) → HCID 67763089, compound

Participants

Reaction Steps

A mixture of 0.24 g of 1-[(4R)-2,2-dimethyl-[1,3]dioxolan-4-ylmethyl]-7-(3-fluoro-4-methoxyphenyl)-1H-pyrazolo[3,4-g]quinoxaline (0.05 g) of pyridinium p-toluenesulfonate and 20 ml of aqueous acetone (1:4H2O:acetone) is heated to reflux overnight. The acetone is then removed in vacuo and the residue mixed with ether, filtered and the yellow solid is treated with saturated NaHCO3, filtered, washed with water and air dried. This is recrystallized from ethylacetate, filtered and dried overnight. This is then recrystallized from CHCl3 and the resultant product purified by column chromatography using 3% MeOH in methylene chloride to obtain 1-[(2R)-1,2-dihydroxyprop-3-yl)-7-(3-fluoro-4-methoxyphenyl)-1H-pyrazolo-[3,4-g]quinoxaline (m.p. 228°-234° C.) and 2-[(2R)-1,2-dihydroxyprop-3-yl)-7-(3-fluoro-4-methoxyphenyl)-2H-pyrazolo-[3,4-g]quinoxaline.

Provenance & Evidence