反应详情

3-nitrophthalic anhydride (0.79 g, 0.0041 mol) and m-aminobenzoic acid (0.56 g, 0.0041 mol) were refluxed as above overnight. Concentration of the solution under vacuum by rotary evaporator and crystallisation of the product from EtOH/H2O yielded 1.23 g (76%) of 126 as a vibrant yellow powder: mp=354-355° C.; Rf0.77 (A): Rf0.84 (C): Rf0.54 (D): IR (cm−1): 2740-3100 (OH), 3088 (C═CH), 2665 (C—H), 1776 (C═O), 1725 (bs, C═O), 1614 (C═C), 1542 (N═O), 1460 (C═C), 1420 (C═C), 1382 (C—O), 1356 (N═O), 1120 (C—O), 717 (C═CH); MS m/z (rel intensity) 311 (100), 267 (65), 191 (60).

1. customConcentration of the solution under vacuum by rotary evaporator and crystallisation of the product from EtOH/H2O