1-Butanol → HCID 68486048, compound

Participants

Reaction Conditions

Reaction Steps

Oleum (25% SO3, 95 ml) is charged into a reactor (350 ml). Under stirring terephthalic acid (19.0 g; 0.11 mol) is added to the reactor and the mixture is heated to 60° C. After stirring for additional 40 min terephthalic acid (31.0 g; 0.19 mol) is added and the mixture is heated to 100° C. for 1 hour. The mixture is cooled to 25-30° C., trioxane (12.0 g; 0.13 mol) is added in portions and the reaction mixture is heated slowly to 120-125° C. and agitated at this temperature for 2 hours and for 4 hours at 145° C. The reaction mixture is cooled to 70° C. and added to a reactor containing butanol (350 ml) which has been heated to 65-70° C. over period of 45 min. The formed precipitates were diluted with butanol (150 ml) and stirring overnight at 40° C. The mixture was heated to reflux for 3 hours, cooled to 50-55° C. and water (500 ml) and heptane (500 ml) were added. The product was filtered off and dried.

Provenance & Evidence