Formaldehyde → HCID 21285052, compound

Participants

Reaction Conditions

Reaction Steps

The process for Example 7 was initiated by charging 593.4 g phenol (6.31 moles) and 0.86 g of triethylamine into a reaction vessel to form a reaction mixture. The reaction mixture was heated to 75° C., and 75.6 g melamine (0.60 moles) was added and mixed for 15 minutes. 53.81 g of 50.17% aqueous formaldehyde (50% of total charge) was added over 30 minutes. 53.61 g of 50.17% aqueous formaldehyde (50% of total charge) was added over 32 minutes. The reaction mixture was maintained at 75° C. for 2 hours and then heated to 85° C. before maintaining the temperature for 30 minutes. The reaction mixture was atmospherically distilled to 110° C. and the temperature was maintained at 110° C. for 3 hours, before reducing the reaction mixture temperature to 100° C. under reflux mode. 4.21 g of benzoic acid slowly over 10 minutes was added and mixed for over 5 minutes. The reaction mixture was then atmospherically distilled to 110° C. and the temperature maintained at 110° C. for 2 hours. The reaction mixture was then atmospherically distilled to 150° C. and the temperature maintained at 150° C. for 2 hours before increasing the temperature to 165° C. while continuing to distill atmospherically. Next, the reaction mixture was under a gradually increasing vacuum over 1.5 hours to full vacuum of at least 27 inches while maintaining a temperature of 163°-165° C. before heating the reaction mixture to 175° C. under full vacuum. Further, the process was concluded by discharging the product (293.6 g) and the vacuum distillate (383.4 g) from the reaction vessel.

Provenance & Evidence