反应详情

To a stirred suspension of 4-cyanomethyl-benzoic acid (1.65 g, 10.24 mmol) and Et3N (5 ml) in pyridine, H2S was bubbled during 3 h. The reaction mixture was stirred 16 h at room temperature. Water was then added to the reaction mixture which was agitated for 1 h before acidifying to pH 6 with 1M HCl. The solvent was evaporated and the residue was triturated 30 min. in water (20 ml) and filtered to obtain the title compound 250 (2.08 g, 83%) as a white solid. 1H NMR (DMSO) δ (ppm): 12.85 (bs, 1H), 9.53 (bs, 1H), 9.43 (bs, 1H), 7.88 (d, J=8.1 Hz, 2H), 7.44 (d. J=8.1 Hz, 2H), 3.88 (s, 2H).

1. customwas bubbled during 3 h
2. additionWater was then added to the reaction mixture which
3. stirringwas agitated for 1 h
4. customThe solvent was evaporated
5. customthe residue was triturated 30 min. in water (20 ml)
6. filtrationfiltered