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 30 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 130-135°C. and agitated at this temperature for 1 1/2 hours and for 4 hours at 155° C. The reaction mixture is cooled to 40° C. and over a period of 30 min added to a reactor containing butanol (300 ml) which has been heated to 95-100° C. Toluene (100 ml) and water (100 ml) was added to the formed suspension. The organic phase was separated and concentrated to dryness and redissolved in toluene (100 ml) and heptanes (100 ml) by heating at 75-80° C. The mixture was cooled to 25-30°C. for 30 min and the product was filtered off and dried.

Provenance & Evidence