A kind of synthetic method of fenbendazole intermediate 2-nitro-4-phenylthioaniline
A technology of phenylthioaniline and fenbendazole, which is applied in the field of synthesis of fenbendazole intermediate 2-nitro-4-phenylthioaniline, can solve the problems of increasing environmental pressure and high yield, and achieves The effect of cost reduction, high yield, and less waste
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Embodiment 1
[0041] Take 25.03g of 2-nitro-4-thiocyanoaniline (purity 95%), add it to a 250mL four-necked flask, add 150.01g of purified water, turn on stirring, rotate speed 300r / min, stir and mix well, this When the solution showed a solid-liquid insoluble yellow-green slurry. Take 30.72g of sodium sulfide nonahydrate and add it to a four-necked bottle, a slight exotherm occurs, the reactant turns into dark purple, and some solids dissolve. The reaction temperature was controlled at 25°C, a small air pump was used, and 0.4 L / min of air was introduced into the reaction system for 1 hour, and a solid was precipitated from the feed liquid. Use a Buchner funnel to filter, and rinse the obtained solid with 50.25g of purified water, and then place it in an airflow oven at 105°C for 4h to obtain 20.40g of an orange-red solid, which is detected as 3,3'-dinitro-4,4', -Diaminodiphenyl disulfide, the detected purity is 98.52%, and the calculated yield is 97.52%.
[0042] Take the above 3,3'-dinit...
Embodiment 2
[0044] Take 25.06g of 2-nitro-4-thiocyanoaniline (purity 95%), add it to a 250mL four-neck flask, add 149.21g of purified water, turn on stirring, rotate speed 300r / min, stir and mix well, this When the solution showed a solid-liquid insoluble yellow-green slurry. Take 32.22g of sodium sulfide nonahydrate and add it to a four-necked bottle, a slight exotherm occurs, the reactant turns into dark purple, and some solids dissolve. The reaction temperature was controlled at 27°C, a small air pump was used, and 0.4 L / min of air was introduced into the reaction system for 1.5 h, and a solid was precipitated from the feed liquid. Use a Buchner funnel to filter, and rinse the obtained solid with 50.12g of purified water, and then put it in an airflow oven at 105°C for 4h to obtain 20.45g of an orange-red solid, which is detected as 3,3'-dinitro-4,4', -Diaminodiphenyldisulfide, the detected purity is 98.88%, and the calculated yield is 98.00%.
[0045] Take the above 3,3'-dinitro-4,4...
Embodiment 3
[0047] Take 24.96g of 2-nitro-4-thiocyanoaniline (purity 95%), add it to a 250mL four-neck flask, add 174.72g of purified water, turn on stirring, rotate speed 300r / min, stir and mix well, this When the solution showed a solid-liquid insoluble yellow-green slurry. Take 29.18g of sodium sulfide nonahydrate and add it to a four-necked bottle, a slight exotherm occurs, the reactant turns into dark purple, and some solids dissolve. The reaction temperature was controlled at 22°C, a small air pump was used, and 0.4 L / min of air was introduced into the reaction system for 1 hour, and a solid was precipitated from the feed liquid. Use a Buchner funnel to filter, and rinse the obtained solid with 50.19 g of purified water, and then place it in an airflow oven at 105 ° C for 4 h to obtain 20.31 g of an orange-red solid, which is detected as 3,3'-dinitro-4,4', -Diaminodiphenyl disulfide, the detected purity is 98.36%, and the calculated yield is 97.21%.
[0048] Take the above 3,3'-di...
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