Industrial production method of acotiamide hydrochloride
The technology of acotiamide hydrochloride and production method, which is applied in the field of medicine and chemical industry, can solve the problems of low purity of acotiamide hydrochloride, unfavorable industrial production and high equipment requirements, and achieves simplified equipment requirements, low production cost and high response. Yield effect
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Example
[0035] (Example 1)
[0036] This example is the preparation method of Intermediate II, which is specifically as follows:
[0037] Add 100L of dichloromethane to a 300L reactor, add 20.95kg of 2,4,5-trimethoxybenzoic acid under stirring, control the temperature at 20-25°C, add 16.22kg of oxalyl chloride dropwise, and finish with about 1.5 drops. The gas (mainly hydrogen chloride, carbon dioxide and a small amount of carbon monoxide) produced during the dripping process is absorbed by the tail gas absorption device, and the reaction liquid is changed from a white turbid liquid to a yellow-green solution. After dripping, slowly add 0.85kg of DMF, about 0.5h to finish, the large amount of gas (mainly hydrogen chloride and carbon dioxide and a small amount of carbon monoxide) generated during the dripping process is absorbed by the exhaust gas absorption device, and the reaction liquid turns into a dark green solution. After dripping, keep the reaction at 20~25℃ for 1h.
[0038] After t...
Example
[0041] (Example 2)
[0042] This example is the preparation method of Intermediate III, which is specifically as follows:
[0043] Add 125L of DMF to a 300L reactor, then add 12.5kg of Intermediate II prepared in Example 1, 11.83kg of pyridine hydrochloride and 5.4kg of pyridine under stirring, and then heat to reflux (about 145~150 ℃), keep stirring and react for 9h, the reaction liquid is brown solution. After the reaction, stop heating and cool to 20-25°C for about 2h.
[0044] Add 210L of water to another 500L reactor, stir and cool to 0-5°C, then slowly add the above reaction liquid into the reactor, stir and crystallize at 15-25°C for 2h, and centrifuge.
[0045] Add 125L of glacial acetic acid and the filter cake obtained after centrifugation to another 300L reactor, stir and heat to reflux (approximately 115-120°C), dissolve, keep warm and stir for 2h. After the reaction, stop heating, cool to 20~25℃, about 2h, then stir for 30min, centrifuge, 40~45℃ vacuum (above 0.080MPa) ...
Example
[0046] (Example 3)
[0047] This embodiment is a preparation method of acotiamide, which is specifically as follows:
[0048] First, prepare a 10wt% sodium carbonate aqueous solution: add 125L of water into a 500L reactor, and then add 12.5kg of Na in four times 2 CO 3 The solid, stir to dissolve, store at 15~25℃ until use.
[0049] Then, 100L of toluene was added to the 300L reactor, 10.00kg of Intermediate III prepared in Example 2 was added with stirring, heated to 70~80℃ with stirring, and then 34.98kg of N,N-diisopropylethylene was added dropwise After dropping the amine, heat to reflux (about 105~110℃), keep the temperature and stir for 4h. After the reaction is over, stop heating, cool down naturally to 20-25℃ (about 2h), then slowly add 50L of glacial acetic acid dropwise, the temperature is controlled not higher than 30℃, after dripping, the pH is 6.0-6.5, and the pH drops to 20 quickly ~25℃.
[0050] Then, 75L of water was added to the reactor, extraction, liquid separatio...
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