Water → Formaldehyde--3,5-dimethylphenol (1/1)

HRID 2295306Notes

Reaction equation

HRID 2295306 reaction equation
[C:1]1([OH:9])[CH:6]=[C:5]([CH3:7])[CH:4]=[C:3]([CH3:8])[CH:2]=1.C(O)(=O)[C:11](O)=[O:12].O>C=O>[C:1]1([OH:9])[CH:6]=[C:5]([CH3:7])[CH:4]=[C:3]([CH3:8])[CH:2]=1.[CH2:11]=[O:12]

Participants

5

Conditions

Temperature
150 °C

Procedure

Into a reactor equipped with a thermometer, an agitator, a reflux cooler and a dropping funnel were charged 122 parts (1 mol) of 3,5-xylenol and 0.6 part of oxalic acid. After the mixture was heated to 150° C., 16.2 parts of 37% aqueous formaldehyde solution was added dropwise to the mixture in two hours, while agitating the resulting mixture without heating. During the dropwise addition of the aqueous formaldehyde solution, the temperature of the reaction system in the reactor was lowered due to the addition of water in the aqueous formaldehyde solution to the reaction system, and the temperature of the reaction system was 102° C. at the final stage of the addition of the formaldehyde solution. The resulting mixture was further agitated at 102° C. for 2 hours and then water was removed from the reaction solution. The residue was charged into a distillation vessel, and unreacted 3,5-xylenol was removed by a distillation under reduced pressure to obtain a 3,5-xylenol/formaldehyde condensate.

Workup

  1. customInto a reactor equipped with a thermometer
  2. temperaturewithout heating
  3. customwas 102° C.
  4. stirringThe resulting mixture was further agitated at 102° C. for 2 hours
  5. customwater was removed from the reaction solution
  6. additionThe residue was charged into a distillation vessel
  7. customunreacted 3,5-xylenol was removed by a distillation under reduced pressure

Sources & evidence

ORD record
ord-4d7d169ebe7c49639d102ed2f363ccaf
Source dataset
uspto-grants-1984_01
Patent number
US04424238

Reaction notes

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