Method for synthesizing 3,3'-dimethyl-4,4'-diamidodiphenylmethane
A technology of diaminodiphenylmethane and dimethyl, applied in the field of organic monomer synthesis, can solve problems such as unsatisfactory product purity, reduced yield, multiple recrystallizations, etc. mild conditions
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Embodiment 1
[0032] A method for synthesizing 3,3'-dimethyl-4,4'-diaminodiphenylmethane, comprising the following process steps:
[0033] a. In a four-necked flask equipped with a stirrer and a thermometer, add 10.7g o-toluidine, and protect it with nitrogen;
[0034] b. 36.5% of 12 g hydrochloric acid was diluted to 50ml with distilled water, the diluted hydrochloric acid was 7.3%, poured into the dropping funnel, added dropwise at a temperature of 15°C, and the dropping time was 0.5 h;
[0035] c. Add 4.06g of formaldehyde with a concentration of 37% dropwise within 0.5h, and react at the same temperature for 1h; then gradually raise the temperature to 55°C within 1.5h, and react for 1h; gradually raise the temperature to 72°C within 0.5h, and react for 2h ;
[0036] d. After the reaction is over, when the temperature is naturally lowered to 35°C, add excess ammonia water dropwise until the pH of the solution is 7, then add potassium hydroxide to adjust the pH of the solution to 9, filt...
Embodiment 2
[0039] A method for synthesizing 3,3'-dimethyl-4,4'-diaminodiphenylmethane, comprising the following process steps:
[0040] a. In a four-necked flask equipped with a stirrer and a thermometer, add 10.7g o-toluidine, and protect with nitrogen;
[0041] b. Dilute 15 g hydrochloric acid of 36.5% to 70ml with distilled water, after dilution, the hydrochloric acid is 6.5%, pour it into the dropping funnel, add dropwise at a temperature of 30°C, and the adding time is 1.5 h;
[0042] c. Add 5.27g of formaldehyde with a concentration of 37% dropwise within 1.5h, and react at the same temperature for 1.5h; then gradually raise the temperature to 60°C within 1h, and react for 1.5h; gradually raise the temperature to 74°C within 0.5h, and react for 3h ;
[0043] d. After the reaction is completed, when the temperature is naturally lowered to 35°C, add excess ammonia water dropwise until the pH of the solution is 8, then add potassium hydroxide to adjust the pH of the solution to 9.5, ...
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