Butylamine → HCID 13732573, compound

Participants

Reaction Steps

2.527 kg (34.5M) n-Butylamine is added to a stirred solution of 23 1 ethanol and 4.58 kg (11,5M) 2-[2-(2-dimethylamino-1-(4-fluorobenzoyl)vinylthio)ethyl]-1,3-isoindoledione under nitrogen atomosphere and the solution is heated at reflux temperature for 24 hours. The reaction mixture is cooled and stirred at 10° for 3 hours. The crude product is collected by filtration, washed several times with ethanol and ether and dried. The crude product is dissolved at 90° in dimethylformamide and the solution is filtered through a heated funnel. A solid begins to form and the resulting suspension is stirred at room temperature overnight, filtered, washed with ether and dried. M.P. 212°-214° ; IR (N): NH 3100, C=O 1580; NMR (DMSO): 7.02-7.55 (m, 6H), 3.48 (m, 2H), 2.77 (m, 2H).

Provenance & Evidence