* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.
(4) 50.0 kg of NE obtained in step (3) was drawn into a reaction kettle, and 25.1 kg of N-methylaniline was drawn in and the temperature was raised to 100 ± 2 C for 15 h.After completion of the incubation, ethanol and N-methylaniline were distilled off under reduced pressure to obtain 62.6 kg of N- (4-ethoxycarbonylphenyl) -N'-methyl-N'-phenylformamidine. The yield was 99.0% (HPLC) 98.0%.The overall yield in four steps was 73.7%.
A mixture of 165 g (1 mol) of ethyl p-aminobenzoate, 112.35 g (1.05 mol) of N-methylaniline, 159 g (1.5 mol) of trimethyl orthoformate and 10.2 g (0.1 mol) of a specific surface area of 137 m2 / g Gamma-type activated alumina into the 500ml reaction flask,Stirring and heating to 50 ~ 60 , incubation reaction 2h. Open the vacuum pump, and gradually increase the vacuum, vacuum distillation of the resulting methanol, to no methanol distillation.The reaction solution was filtered while hot, the recovered active alumina was repeatedly used and the mother liquor was distilled under reduced pressure to give a pale yellow viscous liquid N- (4-ethoxycarbonylphenyl) -N'-methyl-N'-phenyl Formamidine 270 g, yield 95.7%, purity 99.5%.
165 g (1 mol) of ethyl p-aminobenzoate, 117.7 g (1.1 mol) of N-methylaniline, 10 g of p-toluenesulfonic acid,200mL with toluene toluene added to the 1000mL reaction flask, stirred and warmed to 50-60 C, 2h dropwise 59.53g (1.1mol) formic acid(Content of 85%),Heating to reflux reaction, continue to separate the generated water, the reaction of about 5h to stop water when there is no water. The reaction solution was distilled off with atmospheric toluene recovery agent, toluene was recovered, the remaining vacuum distillation reaction solution,A pale yellow viscous liquid N- (4-ethoxycarbonylphenyl) -N'-methyl-N'-phenyl formamidine 262g, yield 93%, purity 99.4%.
With acetic acid; In Petroleum ether; at 50 - 65℃; for 2.25h;Green chemistry;Catalytic behavior;
1) Accurately weigh 16.5 g of ethyl p-aminobenzoate, 16.5 g of trimethyl orthoformate, 16.8 g of N-methylaniline into a 150 mL three-necked flask, and add 60 mL of petroleum ether to a three-necked flask and place it in magnetic stirring. A dropping funnel, a water separator and a thermometer were placed on the three-necked flask, and the outer wall of the water separator was pre-passed with a freezing liquid of -5 C. A three-necked flask was placed in a magnetic stirrer. 2) Stir and raise the temperature to a temperature of 50 C in a three-necked flask .9 g of glacial acetic acid was added dropwise to the reaction vessel within 15 min, and the reaction was kept for 0.6 h; The temperature was raised to 50 C, the reaction was 0.8 h; the temperature was further raised to 65 C, and the reaction was 0.6 h; The liquid in the lower layer of the water separator is continuously separated, and the reflux is stopped at the upper end of the water separator. 3) The reaction mixture was desolvated under a vacuum, then added 60 mL of toluene, cooled to 40 C; 4) Washing 3 times with hydrochloric acid aqueous solution of pH=2, using 50 mL of hydrochloric acid aqueous solution each time, washing for 8 min each time; then washing with 0.6 mol/L sodium bicarbonate aqueous solution 30 mL, adjusting pH to 8; finally washing 3 times with distilled water Every time you use40 mL of distilled water. 5) The organic layer after the water washing treatment was transferred to a rotary steaming flask for vacuum distillation, and the temperature of the vacuum distillation was controlled at about 125 C, and the product was purified by distillation under reduced pressure, the yield was 98%, and the chroma value was 26 Hazen.
With thionyl chloride; In toluene; at 20℃; for 19.5h;
General procedure: 33.8 g (0.25 mol) of N-methylformylaniline, 12.5 g of toluene, and 1.65 g (0.01 mol) of ethyl paraaminobenzoate were added to the reaction device. After stirring and dissolving, 29.8 g of sulfoxide was added dropwise. (0.25 mol), after stirring (about 70 min), continue stirring for 20 min.Then add 225g of toluene, and then add 39.6g (0.24mol) of ethyl p-aminobenzoate step by step. After the addition (about 90min), stir at room temperature for 18h.The material was orange-yellow, and the purity of UV-1 was 93.0% by sampling (HPLC, the same below). The material liquid was heated to 55 ± 1 C and kept for 7 hours. The material liquid was yellow. The purity of UV-1 was 97.3%. Continue heating the material liquid to 90 ± 1 , stop heating, and recover sulfoxide. Cool the recovered sulfoxide to 35 ± 1 , neutralize it with 10wt% sodium carbonate aqueous solution to pH = 6, and control the temperature below 35 . After neutralization, let it stand and separate layers, and layer Desolvation of the organic layer,68.3 g of ultraviolet absorber UV-1 is obtained,The yield was 96.7% and the purity was 99.6%.
Chemistry
Pharmaceutical Intermediates
Inhibitors/Agonists
Material Science
For Research Only
120K+ Compounds
Competitive Price
1-2 Day Shipping
