Acetic Acid → HCID 11449172, compound

Participants

Reaction Conditions

Reaction Steps

A mixture of 45 g of iron powder, 9 ml of acetic acid, and 36 ml of water was heated at 100° C. for 0.5 hour under stirring for activation. To the mixture was added 150 ml of N-methylpyrrolidone. The external temperature was set at 80° C., and 57.2 g of N-(4-chloro-2-fluoro-5-nitrophenyl)phthalimide was added thereto in small portions under stirring (reaction temperature: 85 to 95° C.). After completion of the addition, the stirring was continued at the same temperature for an additional 1 hour period. While the reaction mixture was warm, tetrahydrofuran was added thereto, followed by allowing the mixture to cool. Any insoluble matter was separated by Celite filtration, and the filtrate was concentrated under reduced pressure. Water was added to the concentrate, and the precipitated solid was collected by filtration. The resulting solid was washed successively with water and methanol and dried under reduced pressure to give 48.6 g of the title compound.

Provenance & Evidence