RU2189971C1 - Highly labeled with tritium - Google Patents
Highly labeled with tritium Download PDFInfo
- Publication number
- RU2189971C1 RU2189971C1 RU2001113520A RU2001113520A RU2189971C1 RU 2189971 C1 RU2189971 C1 RU 2189971C1 RU 2001113520 A RU2001113520 A RU 2001113520A RU 2001113520 A RU2001113520 A RU 2001113520A RU 2189971 C1 RU2189971 C1 RU 2189971C1
- Authority
- RU
- Russia
- Prior art keywords
- tritium
- labeled
- highly labeled
- methanol
- organic chemistry
- Prior art date
Links
- 0 Cc1c(Cc(cc2*)cc(C)c2O)c(*)cc(N)c1 Chemical compound Cc1c(Cc(cc2*)cc(C)c2O)c(*)cc(N)c1 0.000 description 2
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
Description
Изобретение относится к области органической химии и может найти применение в аналитической химии, биоорганической химии, биохимии и прикладной медицине. The invention relates to the field of organic chemistry and can find application in analytical chemistry, bioorganic chemistry, biochemistry and applied medicine.
При изучении физиологически активных соединений необходимы их меченые аналоги. When studying physiologically active compounds, their labeled analogues are necessary.
Известен O-(4-гидрокси-3,5-дииодофенил)- 3',5'-дииодо-L-тирозин формулы I:
Данное соединение, получившее наименование "тироксин", является гормональным препаратом (E. Syniewski. //Ann./Thorac.Surg. 1993, v.56, S2-S8;
D.A. Fisher.//Clin.Chem.l996. v.42, p.135-139).Known O- (4-hydroxy-3,5-diiodophenyl) - 3 ', 5'-diiodo-L-tyrosine of the formula I:
This compound, called "thyroxine", is a hormonal drug (E. Syniewski. //Ann./Thorac.Surg. 1993, v.56, S2-S8;
DA Fisher.//Clin.Chem.l996. v. 42, p. 135-139).
Однако его меченный тритием аналог не описан. However, its tritium-labeled counterpart is not described.
Техническим результатом, достигаемым настоящим изобретением, является расширение ассортимента меченых аналогов физиологически активных соединений. The technical result achieved by the present invention is to expand the range of labeled analogues of physiologically active compounds.
Достигается указанный технический результат получением высокомеченного тритием O-(4-гидрокси-3,5-дииодофенил)- 3',5'-дииодо-L-тирозина формулы I. This technical result is achieved by obtaining highly labeled with tritium O- (4-hydroxy-3,5-diiodophenyl) - 3 ', 5'-diiodo-L-tyrosine of the formula I.
Ниже приведен пример реализации изобретения. The following is an example implementation of the invention.
Пример. Example.
В реакционную ампулу помещали 20 мг тироксина, нанесенного на 200 мг катализатора Линдлара. Затем ампулу вакуумировали до давления 0,1 Па, заполняли газообразным тритием до давления 333 гПа и выдерживали при температуре 180oС 10 мин, после чего удаляли избыточный тритий вакуумированием. В ампулу вносили 5 мл метанола, катализатор отфильтровывали, фильтрат упаривали и удаляли лабильный тритий трехкратным упариванием с метанолом. Остаток растворяли в 0,5 мл метанола и меченый препарат выделяли из реакционной смеси методом ВЭЖХ. Выход искомого меченого препарата достигал 20-25%, молярная радиоактивность - 6,5 Kи/ммоль.20 mg of thyroxine supported on 200 mg of Lindlar catalyst were placed in a reaction vial. Then the ampoule was evacuated to a pressure of 0.1 Pa, filled with gaseous tritium to a pressure of 333 hPa and kept at a temperature of 180 ° C. for 10 minutes, after which excess tritium was removed by vacuum. 5 ml of methanol was added to the ampoule, the catalyst was filtered off, the filtrate was evaporated and labile tritium was removed by evaporation three times with methanol. The residue was dissolved in 0.5 ml of methanol and the labeled preparation was isolated from the reaction mixture by HPLC. The yield of the desired labeled preparation reached 20-25%, the molar radioactivity was 6.5 Ki / mmol.
Анализ и очистку меченого препарата проводили высокоэффективной жидкостной (ВЭЖХ) хроматографией (Separon 7 мкм, C18•150 мм, скорость (v) элюента 0,5 мл/мин, в системе 90% метанол - 50 мМ фосфатный буфер (рН 2,8), время удерживания 2,21 мин; в системе 70% метанол - 10 мМ фосфорная кислота, время удерживания 19,21 мин, в системе 75% метанол - 10 мМ фосфорная кислота, время удерживания 24,12 мин, на колонке Silasorb 15 мкм, C18, 10х250 мм, v - 1,0 мл/мин, - 2,0 мл/мин; в системе 85% метанол - 0,2% уксусная кислота - 0,015% трифторуксусная кислота, время удерживания 12,60 мин, на колонке Kromasil 100 С18, 4,6х150 мм; в системе 80% метанол - 10 мМ фосфорная кислота, v - 1,0 мл/мин, - 1,0 мл/мин, время удерживания 2,48 мин).The labeled preparation was analyzed and purified by high performance liquid chromatography (HPLC) (Separon 7 μm, C 18 • 150 mm, eluent speed (v) 0.5 ml / min, in a 90% methanol system — 50 mM phosphate buffer (pH 2.8 ), retention time 2.21 min; in the 70% methanol system - 10 mM phosphoric acid, retention time 19.21 min, in the 75% methanol system - 10 mM phosphoric acid, retention time 24.12 min, on a Silasorb column 15 μm , C 18 , 10x250 mm, v - 1.0 ml / min, - 2.0 ml / min; in the system 85% methanol - 0.2% acetic acid - 0.015% trifluoroacetic acid, retention time 12.60 min, column Kromasil 100 C18, 4,6h150 m; in the system 80% methanol - 10 mM phosphoric acid, v - 1,0 ml / min - 1.0 ml / min, retention time 2.48 min).
Таким образом получено новое высокомеченное тритием физиологически активное соединение. Thus, a new physiologically active compound highly labeled with tritium was obtained.
Claims (1)
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
RU2001113520A RU2189971C1 (en) | 2001-05-22 | 2001-05-22 | Highly labeled with tritium |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
RU2001113520A RU2189971C1 (en) | 2001-05-22 | 2001-05-22 | Highly labeled with tritium |
Publications (1)
Publication Number | Publication Date |
---|---|
RU2189971C1 true RU2189971C1 (en) | 2002-09-27 |
Family
ID=20249729
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
RU2001113520A RU2189971C1 (en) | 2001-05-22 | 2001-05-22 | Highly labeled with tritium |
Country Status (1)
Country | Link |
---|---|
RU (1) | RU2189971C1 (en) |
-
2001
- 2001-05-22 RU RU2001113520A patent/RU2189971C1/en not_active IP Right Cessation
Non-Patent Citations (1)
Title |
---|
Е. Syniewski; Ann. Thorac. Surg.; 1993, v. 56, р.52-58 D.A. Fisher; Clin. Chem.; 1996, v. 42, р.135-139. * |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
JP5604423B2 (en) | Method for preparing Caspofungin and its intermediate | |
JP4468806B2 (en) | Ferrocene compounds and uses thereof | |
RU2189971C1 (en) | Highly labeled with tritium | |
US10036743B2 (en) | Cationic tags for attomole level detection of analytes by mass spectrometry | |
JP2019055921A (en) | Method of producing stereoisomer | |
RU2323224C1 (en) | Tritium uniformly labeled 3h-amphotericin b | |
Ramalingam et al. | An improved synthesis of S-adenosylhomocysteine and related compounds | |
RU2318806C1 (en) | Tritium uniformly labeled [3h]-trans-3,7-dimethyl-9-(2,6,6-trimethyl-3-oxo-1-cyclohexene-1-yl)-2,4,6,8-nonatetraenic acid | |
RU2326889C1 (en) | α-HEDERIN UNIFORMLY MARKED WITH TRITIUM | |
RU2268256C1 (en) | Tritium high-labeled [3h]-(e)-n-[(4-hydroxy-3-methoxyphenyl)methyl]-8-methyl-6-noneneamide | |
RU2233285C1 (en) | Highly tritium labeled [3h]-rapamycin | |
RU2368613C1 (en) | Uniformly tritium-labeled 4,4-difluoro-n-{(1s)-3-[3-(3-isopropyl-5-methyl-4h-1,2,4-triazol-4-yl)-8-azabicyclo[3,2,1]oct-8-yl]-1-phenylpropyl}cyclohexane carbodiimide | |
RU2206562C1 (en) | Highly tritium-labeled 7-(4'-dimethylaminophenyl)-7-oxo-2,4-heptadiene hydroxamic acid | |
RU2265025C1 (en) | Highly labeled with tritium [3h]-2-(imidazol-1-yl)-1-hydroxyethane-1,1-diphosphonic acid | |
RU2351606C1 (en) | Uniformly tritiated triterpene glycosides of holothurians cucumaria | |
RU2291142C1 (en) | 2-AMINO-4-(β-HYDROXYETHYLAMINO)ANISOLE UNIFORMLY LABELED WITH TRITIUM | |
RU2229469C1 (en) | Butyrylcholine chloride highly labeled with tritium | |
RU2197457C1 (en) | High-tritium-labeled n-methyl-n-2-propinylbenzylamine | |
RU2309929C2 (en) | Chlorohexidine highly labeled with tritium | |
RU2291147C2 (en) | [3h]-fluvastatin highly labeled with tritium | |
RU2248965C1 (en) | Tritium highly labeled [3h]-(s)-alpha-cyano-3-phenoxybenzyl-(1r)-(2',2'-dibromovinyl)-2,2-dimethyl cyclopropane carboxylate | |
RU2155175C2 (en) | Tritium highly marked-(2-ano-2-methoxyiminoacetyl)-3- ethylurea | |
RU2190591C1 (en) | 2-methyl-3-phythyl-1,4-naphthoquinone highly labeled with tritium | |
RU2513852C1 (en) | UNIFORMLY TRITIUM-LABELLED PYRO-Glu-His-Pro-NH2 | |
RU2499786C1 (en) | UNIFORMLY LABELLED (3aS, 5S, 6R, 7aR, 7bS, 9aS, 10R, 12aS, 12bS)-10-[(2S, 3R, 4R, 5S)-3,4-DIHYDROXY-5,6-DIMETHYL-2-HEPTANYL]-5,6-DIHYDROXY-7a,9a-DIMETHYLHEXADECANE HYDRO-3H-BENZO [c]INDENO [5,4-e]OXEPIN-3-ONE TRIMER |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
MM4A | The patent is invalid due to non-payment of fees |
Effective date: 20110523 |