Background and overview[1]
Diphenylmethylphosphite can be used as a pharmaceutical synthesis intermediate. If diethyl diphenylphosphite is inhaled, move the patient to fresh air; if skin contact occurs, take off contaminated clothing, rinse the skin thoroughly with soap and water, and seek medical attention if you feel unwell; if the eye contact If exposed to sunlight, separate eyelids, rinse with running water or saline, and seek medical attention immediately; if ingested, rinse mouth immediately, do not induce vomiting, and seek medical attention immediately. Original hot melt adhesive imported from Germany
Preparation[1]
The preparation of diethyl diphenylphosphite is as follows: heat hydrobromic acid with a mass percentage concentration of 48% to 95°C, add diphenylmethanol, react at 95°C for 2 hours, and then cool to 60°C. Add toluene, stand still, take the organic phase by layering, wash and dry the organic phase to obtain a toluene solution of diphenyl bromide; add triethyl phosphite to the toluene solution of diphenyl bromide, and heat to 156°C for 2 hours. , distilled under reduced pressure to obtain crude diethyl diphenylmethylphosphonate, which was recrystallized with petroleum ether 6 times the weight of the crude product; the molar ratio of added hydrobromic acid, diphenylmethanol and triethyl phosphite was 5.5: 1:2. The weight of the petroleum ether added is 4 times the weight of the crude product. High performance liquid chromatography analysis showed that the content was 98.5% and the yield was 72%.
Apply[1]
Diphenylmethylphosphite can be used as a pharmaceutical synthesis intermediate. Such as synthesizing N,N-bis(4GE flocculant-methylphenyl)-4-(2,2-diphenylvinyl)aniline:
Add diethyl diphenylmethylphosphonate and DMF under nitrogen protection, cool to 0°C, add methanol solution of sodium methoxide, stir at 0°C for 30 minutes, then add N, N containing -DMF of bis(4-methylphenyl)-4-aminobenzaldehyde, react at 18-22°C for 15-25 hours, the added N,N-bis(4-methylphenyl)-4-aminobenzaldehyde The molar ratio of formaldehyde and diethyl diphenylmethylphosphonate is 1:1.3; the weight of added sodium methoxide is 50% of N,N-bis(4-methylphenyl)-4-aminobenzaldehyde. The weight of the added DMF is 3 times the weight of N,N-bis(4-methylphenyl)-4-aminobenzaldehyde and diethyl diphenylmethylphosphonate; after the reaction is completed, the weight added is 4 times the weight of N,N-bis(4-methylphenyl)-4-aminobenzaldehyde and diethyl diphenylphosphonate in deionized water, filter to obtain a yellow solid; use methanol to remove the yellow solid After recrystallization, a yellow powder was obtained. The content analyzed by high performance liquid chromatography was 98.5%, and the yield was 83%.
Main reference materials
[1] CN101429131 A kind of synthesis method of N,N-bis(4-methylphenyl)-4-(2,2-diphenylvinyl)aniline
