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A suspension of 13.8 g of 3-nitroaniline and 20 mL of triethylamine in 200 mL methylene chloride was cooled to 0° C. under a nitrogen atmosphere atmosphere and treated with 10.2 g of acetyl chloride, added in a dropwise manner. The reaction mixture was allowed by warm to room temperature overnight. Removal of the volatiles in vacuo gave a crude yellow solid which was washed with 5% aqueous hydrochloric acid, water and was then dried. The yield of 3-nitroacetanilide was 17.4 g as a light yellow solid, m.p. 147°-149° C.; NMR (CDCl3 /DMSO-d6): δ 2.1 (3H, br s), 7.5 (1H, t, J=9 Hz), 8.0 (2H, br t), 8.6 (1H, br s) 10.1 (1H, br s); IR(KBr): 1675, 1550, 1525, 1350 cm-1.

1. additionadded in a dropwise manner
2. temperatureby warm to room temperature overnight
3. customRemoval of the volatiles in vacuo
4. customgave a crude yellow solid which
5. washwas washed with 5% aqueous hydrochloric acid, water
6. customwas then dried