HCID 10737082, compound → HCID 178432042, compound

Participants

Reaction Conditions

Reaction Steps

To a solution of 500 mg 2-(6-acetamido-3,4dihydro-2,2-dimethyl-7-nitro-2H-1,4-benzoxazin-4-yl)pyridine 1-oxide in 10 ml acetic acid, was added 40 mg 10% palladium-carbon to perform catalytic hydrogenation, the reaction mixture was filtered by the use of Celite, and the filtrate was stirred at 100° C. for 30 minutes. After cooling, the solvent was distilled off under reduced pressure, the rest was neutralized by addition of a saturated aqueous solution of sodium bicarbonate and extracted with chloroform, the extract was washed with water and dried over anhydrous magnesium sulfate, and the solvent was distilled off from the dried solution under reduced pressure. The residue thus obtained was purified by column chromatography on silica gel (elutant: 1:1 mixture of chloroform and methanol), and further recrystallized from ethanol-isopropyl ether, thus giving 180 mg of 2-(7,8-dihydro-2,6,6-trimethyl-6H-[1,4]oxazino[2,3-f]benzimidazol-8-yl)pyridine 1-oxide.

Provenance & Evidence