Boron trifluoride etherate → HCID 13376464, compound

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Reaction Steps

22.0 g of N-(2-fluoroacetamido-5-nitrobenzoyl)-2-methyl-4-chloroaniline are dissolved in 170 ml of acetic acid, and 20 g of boron trifluoride etherate are added thereto. The mixture is stirred at 95° to 100° C. for 30 minutes. The mixture is cooled and concentrated under reduced pressure to remove acetic acid. Water is added to the residue and the mixture is neutralized with sodium bicarbonate. The mixture is extracted with chloroform, and the extract is washed with water, dried and then concentrated to dryness under reduced pressure. Isopropanol is added to the crystalline residue and the crystals are collected therefrom. The thus-obtained crystals are recrystallized from a mixture of dimethylformamide and ethanol (1:2). 18.5 g of 2-fluoromethyl-3-(2-methyl-4-chlorophenyl)-6-nitro-4(3H)-quinazolinone are obtained as colorless prisms.

Provenance & Evidence