Hydrochloric Acid → HCID 657140, compound

Participants

Reaction Steps

2N sodium hydroxide (12 ml) was added to a solution of 4-(2-(3-nitrobenzoylamino)-phenoxy)phthalic acid dimethylester (1.15 g, 2.83 mmol) in 1,4-dioxan (12 ml) at room temperature. The mixture was stirred for 2 hours, cooled to <10° C. and pH adjusted to 2-3 with 1N hydrochloric acid (approx. 24 ml). The resulting crystals were filtered off and washed with water. The crystals were dried to give beige crystals of 4-[2-(3-nitrobenzoylamino)-phenoxyl]phthalic acid (yield: 0.82 g. (76%)). 1H—NMR (CDCl3) in ppm: δ 10.3 (s, 1H), 8.38 (m, 1H), 8.18 (d, 1H), 7.6-7.8 (m, 3H), 7.3-7.4 (m, 2H), 7.18 (d.d., 1H), 7.1 (m, 1H), 7.07 (d.d., 1H). Mp: 199.7-201.0° C.

Provenance & Evidence