SU825530A1 - Method of preparing ethylchlorosilanes - Google Patents

Method of preparing ethylchlorosilanes Download PDF

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Publication number
SU825530A1
SU825530A1 SU782688450A SU2688450A SU825530A1 SU 825530 A1 SU825530 A1 SU 825530A1 SU 782688450 A SU782688450 A SU 782688450A SU 2688450 A SU2688450 A SU 2688450A SU 825530 A1 SU825530 A1 SU 825530A1
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USSR - Soviet Union
Prior art keywords
naphthyridine
product
yield
hydroxy
sodium hydroxide
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SU782688450A
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Russian (ru)
Inventor
Александр Евгеньевич Збарский
Леонид Дмитриевич Смирнов
Кирилл Михайлович Дюмаев
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Inst Khim Fiz An Sssr
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Priority to SU782688450A priority Critical patent/SU825530A1/en
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Publication of SU825530A1 publication Critical patent/SU825530A1/en

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Description

(54) СПОСОБ ПОЛУЧЕНИЯ 3-ОКСИ-1,5-НАФТИРИДИНА(54) METHOD FOR OBTAINING 3-OXY-1,5-NAFTYRIDINE

Claims (1)

Изобретение относитс  к усовершеи ствованному способу получени  3-окси -1,5-нафтиридина, который находит пр менение в качестве стимул тора роста растений и в качестве промежуточного продукта в синтезе биологически акти ных соединений. Известен способ получени  3-окси- -1,5-нафтиридина в качестве побочного продукта реакции Скраупа 3,5диаминопиридином . Последний смешиваю с раствором натриевой соли м-нитробензолсульфоновой кислоты в смеси глицерина и 75%-ной серной кислоты. Реакционную массу вьщерживают 3 ч при 135С, по окончании нейтрализу ют до щелочной среды с последующей экстракцией серным эфиром и хроматографированием элюата р Недостатком способа  вл етс  низкий выход 3-окси-1,5-нафтиридина(5,3 Кроме того, выделение его из смеси (З-амино-1,5-нафтиридин; 1,5,7-триазофенантрен и др.) возможно только посредством хроматографировани , что не может быть осуществлено в промышленных масштабах. Цель изобретени  - увеличение выхода целевого продукта. Поставленна  цель достигаетс  тем, что провод т гидролиз 3-бром-1,5-нафтиридина избытком едкого натра в метаноле при 145-155 0. На 1 моль 3-бром-I,5-нафтиридина используют 10 моль едкого натра. Выход целевого продукта 65-70%. Пример. 5г (0,025 М) 3-Бром1 ,5-нафтиридина нагревают в металлической бомбе в растворе 8 г (0,2 М) едкого натра в 40 мл метанола при 145155с в течение 24 ч. Затем реакционную массу фильтруют через слой активированного угл  дл  того, чтобы избавитьс  от частично осмолившегос  продукта. Далее маточник упаривают досуха, раствор ют в воде и нейтрализуют 20%-ной серной кислотой до рН 5. По окончании нейтрализации во3 ду упаривают под вакуумом досуха. Су хой остаток экстрагируют абсолютированным этанолом в экстракторе Сакслета в течение 2 ч. Растворитель отгон ют до начала выпадени  кристаллов. Выход технического продукта 80%. Дл  получени  чистого вещества 3-окси-I ,5-нафтиридин сублимируют при 2 мм рт.ст Сублимированный продукт кристаллизуют,из этанола. Выход чистого продукта 65-70% от теоретического. Т.пл. 280-282 С (281282°С по литературным данным). Предлагаемый способ позвол ет уве личить выход З-окси-1,5-нафтиридина более,чем в 10 раз. 0 Формула изобретени  Способ получени  З-окси-1,5-нафтиридина , отличающийс  тем, что, с целью увеличени  выхода целевого продукта, З-бром-1,5-нафтиридин подвергают гидролизу избытком едкого натра в метаноле при 145155 С . Источники информации, прин тые во внимание при экспертизе 1. Czuba W. Реакци  Скраупа с 3,5-диаминопиридином. - Roczniki Chim 1967, 41, с.289.The invention relates to an improved method for the preparation of 3-hydroxy -1,5-naphthyridine, which is used as a plant growth promoter and as an intermediate product in the synthesis of biologically active compounds. A known method for the preparation of 3-hydroxy -1,5 naphthyridine as a by-product of the Skraup reaction of 3,5-diaminopyridine. The latter is mixed with a solution of the sodium salt of m-nitrobenzenesulfonic acid in a mixture of glycerol and 75% sulfuric acid. The reaction mass is left for 3 hours at 135 ° C, neutralized to an alkaline medium at the end, followed by extraction with sulfuric ether and chromatography of the eluent p. The disadvantage of this method is the low yield of 3-hydroxy-1,5-naphthyridine (5.3) (Z-amino-1,5-naphthyridine; 1,5,7-triazophenanthrene, etc.) is possible only by means of chromatography, which cannot be carried out on an industrial scale. The purpose of the invention is to increase the yield of the target product. hydrolysis of 3-bromo-1,5-on is carried out tyridine with excess sodium hydroxide in methanol at 145-155 0. 10 mol of sodium hydroxide is used per 1 mole of 3-bromo-I, 5-naphthyridine., Yield of the desired product is 65-70% .Example 5g (0.025 M) 3-Brom1, 5 -naphthyridine is heated in a metal bomb in a solution of 8 g (0.2 M) sodium hydroxide in 40 ml of methanol at 145155 s for 24 hours. Then the reaction mass is filtered through a layer of activated carbon in order to get rid of the partially tarred product. Next, the mother liquor is evaporated to dryness, dissolved in water and neutralized with 20% sulfuric acid to pH 5. After neutralization is complete, the water is evaporated under vacuum to dryness. The dry residue is extracted with absolute ethanol in a Saxlet extractor for 2 hours. The solvent is distilled off before the crystals begin to precipitate. The yield of technical product 80%. To obtain pure substance, 3-hydroxy-I, 5-naphthyridine is sublimated at 2 mm Hg. The sublimated product is crystallized from ethanol. The yield of pure product is 65-70% of the theoretical. M.p. 280-282 С (281282 ° С according to literary data). The proposed method allows increasing the yield of 3-hydroxy-1,5-naphthyridine by more than 10 times. 0 Claims of the method of producing 3-hydroxy-1,5-naphthyridine, characterized in that, in order to increase the yield of the target product, 3-bromo-1,5-naphthyridine is subjected to hydrolysis with an excess of sodium hydroxide in methanol at 145155 ° C. Sources of information taken into account in the examination 1. Czuba W. Skraup reaction with 3,5-diaminopyridine. - Roczniki Chim 1967, 41, p.
SU782688450A 1978-11-24 1978-11-24 Method of preparing ethylchlorosilanes SU825530A1 (en)

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SU782688450A SU825530A1 (en) 1978-11-24 1978-11-24 Method of preparing ethylchlorosilanes

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Application Number Priority Date Filing Date Title
SU782688450A SU825530A1 (en) 1978-11-24 1978-11-24 Method of preparing ethylchlorosilanes

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SU825530A1 true SU825530A1 (en) 1981-04-30

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