Hydrochloric Acid → HCID 135845402, compound

Participants

Reaction Steps

148.7 g (1.21 mol) of anhydrous aluminium trichloride (purity 98%) are added with stirring to a suspension of 130.0 g (0.485 mol) of 2-mesityl-4,6-dichloro-1,3,5-triazine (compound 1a) in 300 ml of petroleum ether (boiling range 110°-140° C.) and 385 ml of sulfolane. During this addition, the mixture warms to 45° C. A solution of 133.5 g (1.21 mol) of resorcinol (purity 98%) in 155 ml of sulfolane is added over the course of 45 minutes. The mixture is warmed at 80°-85° C. for 5 hours 30 minutes with evolution of HCl. The upper phase (petroleum ether) is removed, and the lower, viscous phase is transferred while hot into a stirred mixture of 2.1 l of methanol and 2.1 l of water. After the mixture has been stirred for 14 hours, the solid is filtered off, stirred for 1 hour in 2.2 l of 1 molar HCl and filtered off again. The filter cake is suspended in 1000 ml of water, stirred for 30 minutes and re-filtered. This operation is repeated twice. The filter cake is dried for 24 hours at 80° C. and a pressure of 60 mmHg (8000 Pa), giving 170.5 g of the title product (compound 1b) of the formula ##STR104## of m.p. 230°-234° C.

Provenance & Evidence