Ethanol → HCID 178421796, compound

Participants

Reaction Conditions

Reaction Steps

The compound obtained in Example 262 (0.63 g, 2.76 mmol) was dissolved in ethanol (50 ml), to which hydroxylamine hydrochloride (0.38 g, 5.5 mmol) and triethylamine (1.15 ml, 8.3 mmol) were added. The mixture was refluxed with heat at 90° C. for 1 hour. The solvent was distilled off under reduced pressure. To the residue, water and chloroform were added. The precipitate was collected by filtration, and washed with water and chloroform. Subsequently, the washed material was dissolved in hot methanol and chloroform, followed by drying over magnesium sulfate. When the solvent was distilled off under reduced pressure, 0.47 g of the title compound was obtained as a white solid (65%). This solid was recrystallized from methanol--ether to obtain colorless crystals (mp.: 251°-254° C.).

Provenance & Evidence