SU1265193A1 - Method of producing 3-ethoxycarbonylaminepyridine - Google Patents
Method of producing 3-ethoxycarbonylaminepyridine Download PDFInfo
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- SU1265193A1 SU1265193A1 SU853860895A SU3860895A SU1265193A1 SU 1265193 A1 SU1265193 A1 SU 1265193A1 SU 853860895 A SU853860895 A SU 853860895A SU 3860895 A SU3860895 A SU 3860895A SU 1265193 A1 SU1265193 A1 SU 1265193A1
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- SU
- USSR - Soviet Union
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- trichlorethylene
- ethanol
- liters
- producing
- yield
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- Pyridine Compounds (AREA)
Abstract
Изобретение касаетс замещенных пиридинов, в частности получени 3-этоксикарбониламинопиридина (АП), вл ющегос полупродуктом дл синтеза биологически активных веществ. АП получают диазотированием сол нокислого водного раствора гидразида никотиновой кислоты и обработкой полученного азида этанолом в среде трихлорэтилена при 80-90 С до прекращени выделени азота. После отгонки растворител получают АП с 90%-ным выходом и т.пл. 86-88С.The invention relates to substituted pyridines, in particular the preparation of 3-ethoxycarbonylaminopyridine (AP), which is an intermediate for the synthesis of biologically active substances. AP is obtained by diazotization of a hydrochloric aqueous solution of nicotinic hydrazide and treatment of the resulting azide with ethanol in trichlorethylene at 80-90 ° C until the evolution of nitrogen ceases. After distilling off the solvent, AP is obtained in 90% yield, and so forth. 86-88C.
Description
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Изобретение относитс к усовершенствованному способу получени 3-этоксикарбониламинопиридина , который может найти применение как полупродукт дл синтеза биологически активных соединений.The invention relates to an improved process for the preparation of 3-ethoxycarbonylaminopyridine, which can be used as an intermediate for the synthesis of biologically active compounds.
Целью изобретени вл етс повышение выхода 3-этоксикарбониламинопиридина .The aim of the invention is to increase the yield of 3-ethoxycarbonylaminopyridine.
Пример 1. В стекл нном реакторе объемом 20 л раствор ют 2,23 кг гидразида никотиновой кислоты в растворе 3,5 л концентрированной сол ной кислоты в 2 л воды. К полученной смеси в течение 2-3 ч при интенсивном перемешивании и температуре прибавл ют раствор 2,7 кг нитрита натри в 5 л воды, выдерживают 1 ч при и нейтрализуют раствором 1 кг карбоната натри в 5 л воды. Образовавшийс азид экстрагируют из реакционной смеси трихлорэтиленом (ЗчЗ л) и трихлорэтипеновый раствор сушат 1 кг безводного сульфата натри . К сухому раствору азида никотиновой кислоты в трихлорэтилене добавл ют 2 л этанола, после чего нагревают при 85°С до прекращени выделени азота (7,5 ч). Затем из реакционной . массы отгон ют растворитель и избыток спирта. Получают кристаллическоеExample 1 In a glass reactor with a volume of 20 liters, 2.23 kg of nicotinic acid hydrazide was dissolved in a solution of 3.5 liters of concentrated hydrochloric acid in 2 liters of water. A solution of 2.7 kg of sodium nitrite in 5 liters of water is added to the mixture for 2-3 hours with vigorous stirring and temperature. The mixture is kept for 1 hour and neutralized with a solution of 1 kg of sodium carbonate in 5 liters of water. The resulting azide is extracted from the reaction mixture with trichlorethylene (3 × 3 liters) and the trichloro ethylene solution is dried with 1 kg of anhydrous sodium sulfate. To a dry solution of nicotinic acid azide in trichloroethylene, 2 liters of ethanol are added, and then heated at 85 ° C until the evolution of nitrogen ceases (7.5 hours). Then from the reactionary. the masses are distilled off the solvent and excess alcohol. Get crystalline
9393
вещество кремового цвета. Выход 2,2 кг (90%), t. пл. 86-88 с.cream colored substance. Yield 2.2 kg (90%), t. square 86-88 s.
П р и м е р 2. Способ осуществл ют аналогично примеру 1. Раствор азида в трихлорэтилене нагревают с этанолом при 80°С. Вьоделение продукта реакции провод т как в примере 1. Выход 2,0 кг (81%).PRI mme R 2. The method is carried out analogously to Example 1. A solution of azide in trichlorethylene is heated with ethanol at 80 ° C. The separation of the reaction product is carried out as in Example 1. A yield of 2.0 kg (81%).
П р и м е р 3. Способ осуществл ю аналогично примеру 1. Раствор азида в трихлорэтилене нагревают с этанолоPRI me R 3. The method is carried out analogously to example 1. A solution of azide in trichlorethylene is heated with ethanol
при 90°С. Выделение продукта реакций провод т как в примере I. Выход 2,2 кг (90%).at 90 ° C. Isolation of the reaction product is carried out as in Example I. Yield 2.2 kg (90%).
Claims (1)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| SU853860895A SU1265193A1 (en) | 1985-02-25 | 1985-02-25 | Method of producing 3-ethoxycarbonylaminepyridine |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| SU853860895A SU1265193A1 (en) | 1985-02-25 | 1985-02-25 | Method of producing 3-ethoxycarbonylaminepyridine |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| SU1265193A1 true SU1265193A1 (en) | 1986-10-23 |
Family
ID=21164679
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| SU853860895A SU1265193A1 (en) | 1985-02-25 | 1985-02-25 | Method of producing 3-ethoxycarbonylaminepyridine |
Country Status (1)
| Country | Link |
|---|---|
| SU (1) | SU1265193A1 (en) |
-
1985
- 1985-02-25 SU SU853860895A patent/SU1265193A1/en active
Non-Patent Citations (1)
| Title |
|---|
| Clark-Levis J.W., Thompson M.J. Methylation of 3-aminopyridines and preparation of 2-amino-3-methylaminopyridine and ,2,3-diaminopyridine. J. Chem.Soc., 1957, № 1, p.442-446. * |
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