Hydrochloric Acid → HCID 14461232, compound

Participants

Reaction Conditions

Reaction Steps

In a 250 ml of round-bottom three-necked flask, 0.68 g of zinc chloride (dried for 3 hours under vacuum at 100° C.); 4.0 g of 1,3,5-trioxane; 16.0 g of 4-trifluoromethyldiphenylmethane and 4.5 ml of 100% acetic acid are combined, heated to 60° C. and dried halogen chloride gas is introduced. The result is a two phase system that turns brown. HCl was introduced for a total of 3 hours. Following 6 hours of reaction time, the conversion is d.c. controlled (developing agent: petroleum benzin 60°-80° C., result: no conversion, starting material). Once again 0.68 g of ZnCl2 and 2.0 g of 1,3,5-trioxane are added to the reaction mixture and stirred overnight. The reaction mixture was stirred for a total of 30 hours at 60° C., whereby following dc result, approximately 20% of the desired compound formed. The mixture was cooled to room temperature and diluted with 150 ml of diethyl ether. The ether solution was washed to neutral several times with a total of 2.5 liters of water. The organic phase was shaken once with 80 ml of a saturated sodium hydrogen carbonate solution and then washed to neutral 2 times with 90 ml of water each time. The organic phase was dried over sodium sulfate. The drying agent was removed by filtration and the filtrate was concentrated in a rotary evaporator (30° C., water-jet vacuum).

Provenance & Evidence