Hydroxyamine hydrochloride → HCID 88397677, compound

Participants

Reaction Steps

The compound of Example 4 (0.5 g) was dissolved in methanol followed by hydroxylamine hydrochloride (0.220 g) and sodium acetate (0.7 g). The reaction was stirred for 16 hours, the solvent was removed and the residue was dissolved in ethyl acetate (100 ml), washed with water (100 ml), dried (MgSO4), filtered and evaporated to yield an oil which was purified by chromatography on silica using dichloromethane/Et2O (3:1) to yield the title compound isomer A as a white solid, mp=200°-201° C.; found: C, 54.79; H, 4.24; N, 5.19; C23H20F6N2O2S requires C, 54.98; H, 4.01; N, 5.58%. Further elution yielded the title compound isomer B as a white solid, mp=200°-203° C.; found: C, 55.13; H, 4.14; N, 5.45; C23H20F6N2O2S requires C, 54.98; H, 4.01; N, 5.58 %.

Provenance & Evidence