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