SU570603A1 - Method of preparing 2,3,5,6-tetrabromine-4-oxypyridine - Google Patents
Method of preparing 2,3,5,6-tetrabromine-4-oxypyridineInfo
- Publication number
- SU570603A1 SU570603A1 SU7602351547A SU2351547A SU570603A1 SU 570603 A1 SU570603 A1 SU 570603A1 SU 7602351547 A SU7602351547 A SU 7602351547A SU 2351547 A SU2351547 A SU 2351547A SU 570603 A1 SU570603 A1 SU 570603A1
- Authority
- SU
- USSR - Soviet Union
- Prior art keywords
- hydroxypyridine
- tetrabromine
- oxypyridine
- preparing
- yield
- Prior art date
Links
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Description
1one
Изобретение относитс к улучшенному способу получени 2,3,5,6-тетрабром-4-оксипиридина - ценного промежуточного продукта дл синтеза различных производных полибромпиридинов .This invention relates to an improved process for the preparation of 2,3,5,6-tetrabromo-4-hydroxypyridine, a valuable intermediate for the synthesis of various polybromopyridine derivatives.
Известен способ получени 2,3,5,6-тетрабром-4-оксипиридина , заключающийс в том, что 3,5-дибром-4-оксипиридина нагревают в течение 120 ч с бромом в 70%-ном олеуме. Выход целевого продукта 85% 1.A method of producing 2,3,5,6-tetrabromo-4-hydroxypyridine is known, which consists in that 3,5-dibromo-4-hydroxypyridine is heated for 120 hours with bromine in 70% oleum. The yield of the target product is 85% 1.
Исходный 3,5-дибром-4-оксипиридин получают с выходом 30-40% в результате бромировани 4-оксипиридина бромной водой 2.The starting 3,5-dibromo-4-hydroxypyridine is obtained in a yield of 30-40% by brominating the 4-hydroxypyridine with bromine water 2.
Целью изобретени вл етс упрощение процесса и увеличение выхода целевого продукта .The aim of the invention is to simplify the process and increase the yield of the target product.
Это достигаетс бромированием 4-оксипиридина в 80%-ном олеуме, в результате чего получают 2,3,5,6-тетрабром-4-оксипиридин с 75%-ным выходом.This is achieved by brominating 4-hydroxypyridine in 80% oleum, resulting in 2,3,5,6-tetrabromo-4-hydroxypyridine in 75% yield.
Такой способ дает возможность получить целевой продукт с более высоким выходом в пересчете на исходный 4-оксипиридин, сократив при этом одна дополнительна стади сокращаетс ..:This method makes it possible to obtain the target product with a higher yield in terms of the initial 4-hydroxypyridine, while reducing one additional step is reduced ..:
Пример. 2,3,5,6-Тетрабром-4-оксипириДин .Example. 2,3,5,6-Tetrabrom-4-oxypiriDine.
К смеси, приготовленной при температуре - 10°С из 40 г (0,421 моль) 4-оксипиридина и 50 мл серной кислоты (d 1,84), прибавл ют 1000 мл 85%-него олеума. Реакционную смесь при перемешивании (затвор из тефлонового унлотнител ) выдерживают 85 ч при 80°С, добавл 80 мл сухого брома порци ми по 20 мл в первые 20 ч и 50 мл брома порци ми по 10 мл в последующие 40 ч. Избыток брома отдел ют и реакционную смесь выливают на лед. Продукт отфильтровывают, промывают водой и сушат.To a mixture prepared at a temperature of -10 ° C out of 40 g (0.421 mol) of 4-hydroxypyridine and 50 ml of sulfuric acid (d 1.84) was added 1000 ml of 85% oleum. The reaction mixture was stirred for 85 hours at 80 ° C with stirring (shutter from a Teflon container), adding 80 ml of dry bromine in 20 ml portions in the first 20 hours and 50 ml bromine in 10 ml portions in the next 40 hours. Excess bromine was separated and the reaction mixture is poured onto ice. The product is filtered, washed with water and dried.
Выход 129,8 г (75%); т. пл. 256-257°С (из уксусной кислоты).Yield 129.8 g (75%); m.p. 256-257 ° C (from acetic acid).
Найдено,:%: Вг 77,62; N 3,28.Found,:%: Br 77.62; N 3.28.
C5HBr4NO.C5HBr4NO.
Вычислено, %: Вг 77,85; N 3,40.Calculated,%: Br 77.85; N 3.40.
Claims (2)
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
SU7602351547A SU570603A1 (en) | 1976-04-21 | 1976-04-21 | Method of preparing 2,3,5,6-tetrabromine-4-oxypyridine |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
SU7602351547A SU570603A1 (en) | 1976-04-21 | 1976-04-21 | Method of preparing 2,3,5,6-tetrabromine-4-oxypyridine |
Publications (1)
Publication Number | Publication Date |
---|---|
SU570603A1 true SU570603A1 (en) | 1977-08-30 |
Family
ID=20658328
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
SU7602351547A SU570603A1 (en) | 1976-04-21 | 1976-04-21 | Method of preparing 2,3,5,6-tetrabromine-4-oxypyridine |
Country Status (1)
Country | Link |
---|---|
SU (1) | SU570603A1 (en) |
-
1976
- 1976-04-21 SU SU7602351547A patent/SU570603A1/en active
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