SU657031A1

SU657031A1 - Method of obtaining selencyclohexane

Info

Publication number: SU657031A1
Application number: SU772494941A
Authority: SU
Inventors: Эркин Шамхал Оглы Мамедов; Султан Бахшали Оглы Курбанов; Роберт Данилович Мишиев; Тогрул Неймат оглы Шахтахтинский
Original assignee: Институт Теоретических Проблем Химической Технологии Ан Азербайджанской Сср
Priority date: 1977-06-09
Filing date: 1977-06-09
Publication date: 1979-04-15

Description

(54) СПОСОБ ПОЛУЧЕНИЯ СЕЛЕНОЦИКЛОГЕКСАНА(54) METHOD FOR OBTAINING SELENOCYCLOGEXANE

II

Изобретение относитс к усовершенствованному способу получени селеноциклогексана , обладающего физиологической активностью.The invention relates to an improved method for the preparation of selenocyclohexane with physiological activity.

Известен способ получени селеноциклогексана , заключающийс в том, что oL,LO -дихлорпентан подвергают взаимодействию с диселенидом натри при 1ОО С в присутствии катализатора-ронгалита. Выход целевого продукта составл ет 51% l. Недостатком способа вл етс его многостадийность и труднодоступность исходных продуктов.A known method for producing selenocyclohexane is that oL, LO-dichloropentane is reacted with sodium diselenide at 1OO C in the presence of a rongalite catalyst. The yield of the target product is 51% l. The disadvantage of this method is its multi-stage and inaccessibility of the original products.

Целью изобретени вл етс упроще- ние процесса.The aim of the invention is to simplify the process.

Поставленна цель достигаетс описываемым способом получени селеноцикпогексана на основе селенсодержащего соединени при нагревании в присутствии катализатора, заключающимс в том, что в качестве селенсодержащего соединени используют двуокись селена, которую подвергают взаимодействию с н-пентаном при 450-560 С, а в качестве катализатора используют цеолитсодержаший катализатор с редкоземельными элементами- цеокар-2. Процесс предпочтительно проThe goal is achieved by the described method of producing selenocycpohexane based on selenium-containing compound by heating in the presence of a catalyst, which is that selenium dioxide is used as selenium-containing compound, which is reacted with n-pentane at 450-560 ° C, and zeolite-containing catalyst is used as catalyst with rare-earth elements-ceokar-2. The process is preferably about

вод т при 5ОО-52О С. Выход селеноциклогексана составл ет 5-14 вес.%. на пропущенный н-пентан.. Процесс ведут в трубчатом реакторе проточного типа над стационарным слоем катализата. Не вступивший в реакцию н-пентан можно снова возвращать в цикл. Продолжительность действи катализатора составл ет 45 ч.water at 5OO-52 ° C. The yield of selenocyclohexane is 5-14% by weight. on the missed n-pentane .. The process is carried out in a tubular flow-type reactor over a fixed bed of catalyzate. Unreacted n-pentane can be recycled again. The duration of the catalyst is 45 hours.

Пример 1. Трубку из пирекса с внутренни диаметром 16 мм и длиной 600 мм заполн ют 35 г прокален-Example 1. A pyrex tube with an inner diameter of 16 mm and a length of 600 mm is filled with 35 g of calcined

Claims

at ZOO-350 ° C, zeocar-2 and 30 g of selenium dioxide. Then, rising to a temperature of 50 ° -52 ° C, 20 g of n-pentane are fed into the reaction zone along with a stream of nitrogen at a rate of 8 g / h. The catalyst in the amount of 24.7 g collected in the receiver, cooled with dry ice). The organic layer is separated from the aqueous, dried with 2 g of K, CO, and after distillation, the non-propag- ;;; .- g-. .... 6 rovavponon-penoane, the reaction product is twice distilled at atmospheric pressure in a Klysen flask. The composition of the distillation I. g: I fraction (34-35 ° C / | 15 (n-pentane / 760 mm Hg) P fraction (155-162 ° C / / 760 mm Hg) 7, O Residue1 , 2 (pitch) Losses1 5 After the second distillation of fraction D in an amount of 7 g, the desired product is isolated with a boiling point of 159–160 ° C / 760 mm. 6, 0 g (14 wt.%) For the missing tan) or 58.2% for the reacted n-pentane. 1.5448, d | ° 1.3957. The balance of O, 6 g, loss of 0.4, 82, MR ,, 34,23. Example 2. The experiment was carried out under conditions analogous to example 1. From 20 n-pentane at 550-560 ° C, 2, -5 g {5. wt.% on the missed n-penta selenocyclohexane. Return of n-pentane 14 g, residue 2.8 g, loss 2 g. Example 3. The test was carried out under conditions similar to example 1. From 2O g of n-pentane, 4 g was obtained at C (8 wt.% For the missed n-pentane) selenocyclohexane. Return of n-pentane 16 g ,, residue 0.5 g, loss 1.5 g. Invention 1, Method for producing selenocyclohexane based on selenium-containing compound - NIN when heated in the presence of a catalyst, characterized in that, in order to simplify the process , selenium dioxide is used as a selenium-containing compound, which is reacted with n-pentane at 450-560 ° C, and a zeolite-containing catalyst with rare-earth elements, ceokar-2, is used as a catalyst.

2. The method according to claim 1, characterized in that the process is carried out at 50 ° -520 ° C. Sources of information | 1, taken into account during the examination 1. T.V. MeSiEEEi b and .jsfohn Jnofgbn .Chej-n. , 1966, 5, No. 1, p. 15O151.