Formaldehyde → HCID 69677332, compound

Participants

Reaction Conditions

Reaction Steps

A one liter flask was charged with 244.7 g phenol (2.6 moles) and 86.1 g 50% formalin (1.44 moles). The reaction mixture was heated to 60° C. and then 85.8 g N-methylaniline (0.8 mole) and added over 30 minutes at 60° C. The temperature was lowered to 50° C. and 86.1 g 50% formalin (1.44 moles) quickly added. The temperature was raised to 55° C. and than 85.7 g N-methylaniline (0.8 mol) added over 32 minutes at 55-60° C. After 20 minutes at 60° C. the temperature raised to 100° C. and maintained at 100° C. for one hour. Reaction mixture was then atmospherically distilled to 160° C. to collect 136.8 g distillate. Phenol (56.3 g) was then recovered by vacuum distillation increasing temperature to 190° C. while increasing vacuum to 30 inches of mercury. Vacuum was broken and 100 ml deionized water added over 40 minutes at about 190° C. Vacuum was then applied to remove water at 190° C. under 30 inches of mercury. Product yield was 372 g and is characterized in Table 3B and Table 5.

Provenance & Evidence