SU558863A1 - Coordination nitrogenyl ruthenium and method for its preparation - Google Patents
Coordination nitrogenyl ruthenium and method for its preparationInfo
- Publication number
- SU558863A1 SU558863A1 SU2025287A SU2025287A SU558863A1 SU 558863 A1 SU558863 A1 SU 558863A1 SU 2025287 A SU2025287 A SU 2025287A SU 2025287 A SU2025287 A SU 2025287A SU 558863 A1 SU558863 A1 SU 558863A1
- Authority
- SU
- USSR - Soviet Union
- Prior art keywords
- ruthenium
- nitrogenyl
- coordination
- preparation
- hydrated
- Prior art date
Links
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 title claims description 8
- 229910052707 ruthenium Inorganic materials 0.000 title claims description 8
- 238000000034 method Methods 0.000 title claims description 4
- 238000002360 preparation method Methods 0.000 title description 3
- 150000001875 compounds Chemical class 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 3
- NNFCIKHAZHQZJG-UHFFFAOYSA-N potassium cyanide Chemical compound [K+].N#[C-] NNFCIKHAZHQZJG-UHFFFAOYSA-N 0.000 claims description 3
- 239000003054 catalyst Substances 0.000 claims description 2
- 229940088597 hormone Drugs 0.000 claims 1
- 239000005556 hormone Substances 0.000 claims 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 8
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 description 2
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 239000006071 cream Substances 0.000 description 2
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- VZGDMQKNWNREIO-UHFFFAOYSA-N tetrachloromethane Chemical compound ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 description 2
- 238000003776 cleavage reaction Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 238000002329 infrared spectrum Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 239000006193 liquid solution Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229910017464 nitrogen compound Inorganic materials 0.000 description 1
- 150000002830 nitrogen compounds Chemical class 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 150000002978 peroxides Chemical class 0.000 description 1
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical group [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000011541 reaction mixture Substances 0.000 description 1
- YAYGSLOSTXKUBW-UHFFFAOYSA-N ruthenium(2+) Chemical compound [Ru+2] YAYGSLOSTXKUBW-UHFFFAOYSA-N 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 230000007017 scission Effects 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- -1 transition metal salts Chemical class 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/082—Compounds containing nitrogen and non-metals and optionally metals
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
Description
(54) КООРДИНАЦИОННЫЙ РУТЕНИЯ И СПОСОБ ЕГО ПОЛУЧЕНИЯ(54) COORDINATION RUTENIA AND METHOD FOR ITS OBTAINING
II
Изобретение относитс к получению коорданацнинньзх соединений рутени с молекул рным азотом и может найш п{Я менеш1е в качестве каташсзатора р да xHNffiqecKBX нртн ессов.The invention relates to the preparation of coordinated compounds of ruthenium with molecular nitrogen and can be found as a catcher of the xHNffiqecKBX range in the National Trade Union.
Известны нитрогенилышю комплексы элементов платиновой груптл, юлу%иные пр мым П1мсоедние1шем азота прл восстановлении солей переходных металлов в водных раствсфах и ко женцым путем, когда N7 (разуетс непосредственно в коорд шационной сфере, причем источниками азота могут быть гидражн или азщи.Nitrogenic complexes of elements of the platinum group, nitrogen and other direct nitrogen compounds are known to reduce the transition metal salts in aqueous solutions and coagulated, when N7 (developed directly in the coordinate sphere, and nitrogen sources can be hydrated or nitrogen.
В частнссти, дл рутени известны ксн шлексы состава tRu(NH3)5N j Х2,где Хравен С1, 8г, . Эти соединени были получены при взаимодействии солей RU (1П) и (IV) с гидратом гидразина (1.In particular, for ruthenium, xR pulleys of the composition tRu (NH3) 5N j X2 are known, where Heraven C1, 8d,. These compounds were obtained by the interaction of RU (1P) and (IV) salts with hydrazine hydrate (1.
Цель изобретени - получение координадаонного нитрогенила рутени Кз {Ru(CN) 5 N2 SHj дл использовани в качестве катализатора.The purpose of the invention is the preparation of coordinated nitrogenyl ruthenium Cs {Ru (CN) 5 N2 SHj for use as a catalyst.
Координационный нитрогенил рутени общей формулы Кз RU (CN) 5 Nj) 3 Н, О представл ет собой кг емовый с розовым оттенком мелкокртсталлический порошок, хорошо растворимый в воде, но не растворимый в таких органических растворител х, как эфир, метанол, этанол, ацетон, четыреххлористьш углерод, ацетонитрил и др. Coordination nitrogenyl ruthenium of the general formula Kz RU (CN) 5 Nj) 3 H, O is a pink crystalline powder that is well soluble in water but not soluble in organic solvents such as ether, methanol, ethanol, acetone , carbon tetrachloride, acetonitrile, etc.
устойчиво при комнатнсж температуре, тер ет кристаллиза даонную воду при 100-105 С, начало отщеплени молекул рного азота зафиксировано при (. Иншгаидуалыюсть соединени подтверждена рентгенографически, на рентгаюграмме наблюдаютс собственные наборы интер ренций . В ИК-спектре в области 204О-2170 обнаружаи ишрока 1штенснвна полоса, обусловленна колебани ми св зей и , причем на основании ссиюставлеюю с соед1шеннем (RU(NHs)5 Nj) Cli высказываетс предположение, что вьюокочастотные ко вюненты 2110 -2170 см соответствуют валентным колебаш1 м молекулы NJ, а v (CN) про вл ютс при 2040-2080см . Интенсивна и средней интенсивности полосы при 570-550 и 475 отнесены со ответственно к частотам валентных колебаний (RuC+RuN)H (RuNj). : stably at room temperature, loses crystallization water at 100–105 ° C, the onset of molecular nitrogen cleavage was recorded at (The compound’s intrusion was confirmed by X-ray diffraction, its own sets of interferences were observed on the X-ray pattern. In the IR spectrum in the 204O-2170 region, the 1 str the band due to the vibrations of the links and, and on the basis of the connection with the connection (RU (NHs) 5 Nj) Cli, it is assumed that the twofold coyenters of 2110-2110 cm correspond to the stretching vibrational of the molecule NJ, and v (CN) appear at 2040–2080 cm. The intense and medium intensity bands at 570–550 and 475 are related, respectively, to the stretching vibration frequencies (RuC + RuN) H (RuNj).
Способ получени соединени состоит в том что исходное соединение-гидроксотрихлорид рутени - обрабатывают гидратом гидразина в водном растворе при 90-95° С в присутствии цианистого кали с. последующим введением перекиси водорода.The method of preparing the compound is that the starting compound, ruthenium hydroxotrichloride, is treated with hydrazine hydrate in an aqueous solution at 90-95 ° C in the presence of potassium cyanide. the subsequent introduction of hydrogen peroxide.
n р м в p. 4,76 г RuOHdi раствор ют в мпшмшьном колввчестве воды (5 мл), к раствору по кашмм при посто нном перемеишваии прилишают 10 мл П ;ф«та niApaainia. После нэменени коричневой окраски ва темио-крашую ввод т 4 г сухого KCN и реакфо ную нагревают при 90-95 С в течеюм 1,5 час.n p m in p. 4.76 g of RuOHdi is dissolved in water in a mixture (5 ml), and 10 ml of P; fi-ta niApaainia is added to a solution of cachyms at constant mixing. After the brown color is not changed, 4 g of dry KCN are introduced into the temo-aspirinum and the reaction mixture is heated at 90-95 ° C for 1.5 hours.
По мере охлаждени из раствора выпадают рко красные кртсталлы цнаногндразинового комплекса рутени (II) сгютава К, (Ru(CN)4 (N)H4) ) 2НзО.As the cooling proceeds, the bright red crystals of the cyanogndrazine ruthenium (II) complex fall out of the solution, Cgгtava K, (Ru (CN) 4 (N) H4)) 2HzO.
При действии на водный раствор дигндразинотетрашанорутената (II) салк 3% перекиси, водорода (HjOj) и нагревший () на ррот жент 30 мин (жраска раствсфа становитс бледно-роэюой. Из oxnaxQieHHtMo раствора выпадают кремовые с розовым оттенком 1мегвс е кристаллы, хи.Апвский аввлнз кото{шх позвол ет прш:исатъ им формулуUnder the action of an aqueous solution of digndrazinotetrashtrautenat (II), salk 3% peroxide, hydrogen (HjOj) and heated () to the mouth of the jent for 30 minutes (the liquid solution becomes pale red. From the oxnaxQieHHtMo solution, a cream with a pink tinge 1Mg of cream is applied. avvlnz coto {shh allows prsh: use their formula
К, (Ru(CN),Nal«3H30 Найцено,%: Ru 23,65; N 24,81; HjO 12,76. K3lRu(CN)jN,°3HaO Вычислено, %: Ru 23,53; N 24,11; HjO 12,54. М.масса 430.41.K, (Ru (CN), Nal "3H30 Naiceno,%: Ru 23.65; N 24.81; HjO 12.76. K3lRu (CN) jN, ° 3HaO) Calculated,%: Ru 23.53; N 24, 11; HjO 12.54. M.mass 430.41.
Claims (2)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| SU2025287A SU558863A1 (en) | 1974-05-17 | 1974-05-17 | Coordination nitrogenyl ruthenium and method for its preparation |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| SU2025287A SU558863A1 (en) | 1974-05-17 | 1974-05-17 | Coordination nitrogenyl ruthenium and method for its preparation |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| SU558863A1 true SU558863A1 (en) | 1977-05-25 |
Family
ID=20584870
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| SU2025287A SU558863A1 (en) | 1974-05-17 | 1974-05-17 | Coordination nitrogenyl ruthenium and method for its preparation |
Country Status (1)
| Country | Link |
|---|---|
| SU (1) | SU558863A1 (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4309311A (en) | 1980-01-08 | 1982-01-05 | Phillips Petroleum Company | Ammonia synthesis with catalyst derived by heating on a support a salt selected from alkali metal, alkaline earth metal, iron and cobalt hexacyanocobaltates and hexacyanoruthenates |
| US4348370A (en) | 1980-01-08 | 1982-09-07 | Phillips Petroleum Company | Ammonia synthesis with catalyst derived by heating on a support a salt selected from alkali metal, alkaline earth metal, iron and cobalt hexacyanocobaltates and hexacyanoruthenates |
-
1974
- 1974-05-17 SU SU2025287A patent/SU558863A1/en active
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4309311A (en) | 1980-01-08 | 1982-01-05 | Phillips Petroleum Company | Ammonia synthesis with catalyst derived by heating on a support a salt selected from alkali metal, alkaline earth metal, iron and cobalt hexacyanocobaltates and hexacyanoruthenates |
| US4348370A (en) | 1980-01-08 | 1982-09-07 | Phillips Petroleum Company | Ammonia synthesis with catalyst derived by heating on a support a salt selected from alkali metal, alkaline earth metal, iron and cobalt hexacyanocobaltates and hexacyanoruthenates |
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