3-Aminophenol → HCID 69049437, compound

Participants

Reaction Steps

To a 80 ml of anhydrous N,N-dimethylformamide suspension containing 2.18 g of sodium hydride (55 wt %) was added 5.45 g of 3-aminophenol, and the mixture was stirred at room temperature for 20 minutes. Subsequently, 14.3 g of N-(5-chloro-2-nitrophenyl)-N-methylcarbamic acid t-butyl ester (Japanese Patent Application (Kokai) No. Hei 11-193276) was added in small amounts, and the mixture was stirred at 100° C. for 6 hours. The reaction mixture was concentrated, followed by addition of water and neutralization using 3N hydrochloric acid and sodium bicarbonate powder. The insoluble product which deposited was filtered, washed with water, and then dried under reduced pressure to give the title compound (16.6 g, 92% yield).

Provenance & Evidence