2-Chloroaniline → N1,N1-Dimethyl-N2-(o-chlorophenyl)formamidine

Participants

Reaction Steps

98% 2-chloroaniline (195 g; 1.5 mol) and 98% dimethylformamide dimethyl acetal (228.2 g; 1.8 mol) were dissolved in toluene (300 g), and the solution was heated under reflux for 4 h. During this time, the internal temperature fell from 96 to 77° C. Thereafter, 15 g of distillate were removed, and the internal temperature rose again during this time to 84° C. Finally, the reaction solution was concentrated on a rotary evaporator at 90° C. and 5 mbar and the resulting brown oil (270.5 g) was fractionated by means of column distillation. The main fraction distilled over at 120° C. and 1.4 mbar and comprised the product in a purity of >99% (determined using area percentages of the GC spectrum).

Provenance & Evidence