2,6-Lutidine → HCID 21113542, compound

Participants

Reaction Conditions

Reaction Steps

64.8 g (0.641 mol) of sulfur trioxide were added as a 57% solution in 1,2-dichloroethane at from 0 to 5° C. with stirring within 15 minutes to a solution of 90.6 g (0.846 mol) of 2,6-lutidine in 200 ml of 1,2-dichloroethane, followed by washing with 40 ml of 1,2-dichloroethane and stirring for 15 minutes until the temperature had risen to 22° C. Subsequently, 42.4 g (0.385 mol) of N-allyl-N-(2-cyanoethyl)amine were added at from 20 to 30° C. with stirring within 15 minutes, followed by washing with 40 ml of 1,2-dichloroethane and stirring at 50° C. for 15 minutes. After cooling to 22° C., 70.8 g (0.61 mol) of phosphorus oxychloride were added with stirring at from 20 to 30° C. within 15 minutes, followed by washing with 120 ml of 1,2-dichloroethane and heating to 70° C. After stirring at this temperature for 1 hour, the reaction mixture was allowed to cool to 25° C., concentrated under reduced pressure and distilled through a Normag column head with a 10 cm column. 32.3 g (40% of theory) of the title compound with a b.p. of from 110 to 116° C./0.4 mbar were obtained. Refractive index: nD23=1.4948.

Provenance & Evidence