SU173746A1 - METHOD OF OBTAINING SWITCHED 0-METHYLISOM UREE-Y15 - Google Patents
METHOD OF OBTAINING SWITCHED 0-METHYLISOM UREE-Y15Info
- Publication number
- SU173746A1 SU173746A1 SU932449A SU932449A SU173746A1 SU 173746 A1 SU173746 A1 SU 173746A1 SU 932449 A SU932449 A SU 932449A SU 932449 A SU932449 A SU 932449A SU 173746 A1 SU173746 A1 SU 173746A1
- Authority
- SU
- USSR - Soviet Union
- Prior art keywords
- methylisom
- uree
- switched
- obtaining
- urea
- Prior art date
Links
- RTZKZFJDLAIYFH-UHFFFAOYSA-N diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N HCl Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- VAYGXNSJCAHWJZ-UHFFFAOYSA-N Dimethyl sulfate Chemical compound COS(=O)(=O)OC VAYGXNSJCAHWJZ-UHFFFAOYSA-N 0.000 description 3
- OXNIZHLAWKMVMX-UHFFFAOYSA-N Picric acid Chemical compound OC1=C([N+]([O-])=O)C=C([N+]([O-])=O)C=C1[N+]([O-])=O OXNIZHLAWKMVMX-UHFFFAOYSA-N 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 229940075930 picrate Drugs 0.000 description 3
- OXNIZHLAWKMVMX-UHFFFAOYSA-M picrate anion Chemical compound [O-]C1=C([N+]([O-])=O)C=C([N+]([O-])=O)C=C1[N+]([O-])=O OXNIZHLAWKMVMX-UHFFFAOYSA-M 0.000 description 3
- 229940114148 picric acid Drugs 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 229950002929 trinitrophenol Drugs 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 239000000706 filtrate Substances 0.000 description 2
- RMAHPRNLQIRHIJ-UHFFFAOYSA-N methyl carbamimidate Chemical compound COC(N)=N RMAHPRNLQIRHIJ-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- XSQUKJJJFZCRTK-UHFFFAOYSA-N urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- 230000002378 acidificating Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 229910000099 calcium monohydride Inorganic materials 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 238000004949 mass spectrometry Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
Description
Изобретение относитс к области получени меченых по азоту соединений.The invention relates to the field of producing nitrogen-labeled compounds.
Предложенный способ состоит в том, что меченую мочевпну-Nl подвергают взаимодействию с диметилсульфатом при нагревании до 120°С. Выход составл ет 40-50%.The proposed method consists in the fact that the labeled urea-Nl is reacted with dimethyl sulfate when heated to 120 ° C. The yield is 40-50%.
Пример. Смесь, содержащую 6 вес. ч. мочевийы-N I (N13 11,5 ат. о/о) и 25 вес. i. диметилсульфата, медленно «агревают (со скоростью 4-5 град/мин) до 120°С при перемешивании и выдерживают при ПО- 120°С (не выше) еще 40 мин. Затем смесь выливают в гор чий насыщенный водный раствор пикриновой кислоты (34 вес. ч.), став т на короткое врем в холодильник и отфильтровывают выпавший пикрат о-метилизбмочевины-Ы 2 Example. A mixture containing 6 wt. including urea-N I (N13 11.5 at. o / o) and 25 wt. i. dimethyl sulfate, slowly “agglomerated (at a rate of 4–5 deg / min) to 120 ° C with stirring and kept at –– 120 ° C (not higher) for another 40 min. The mixture is then poured into a hot saturated aqueous solution of picric acid (34 parts by weight), placed in a refrigerator for a short time, and the precipitated picrate of o-methyl isothermic acid is filtered off.
Полученный осадок раствор ют в минимальном количестве кип щей воды (400 мл) и добавл ют концентрированной сол ной кислоты до сильно кислой реакции по конго. При этом выпадает пикринова кислота. Смесь охлаждают, отфильтровывают пикриновую кислоту и фильтрат экстрагируют 3- 4 раза эфиром до почти бесцветногораствора . Раствор упаривают в вакууме досуха, прибавл небольшое количество воды, а затем эфир с целью удалени избытка сол ной кислоты. После удалени избытка НС1 вещество выпадает под эфиром. Его отфильтровывают , а фильтрат вновь упаривают в вакууме досуха и получают дополнительное количество вещества. Общий выход хлоргидрата о-метилизомочевины 4,7-5,7 г (40-50% or теоретического, счита на мочевину).The resulting precipitate is dissolved in a minimum amount of boiling water (400 ml) and concentrated hydrochloric acid is added to a highly acidic congo reaction. At the same time falls picric acid. The mixture is cooled, picric acid is filtered off and the filtrate is extracted 3 to 4 times with ether to an almost colorless solution. The solution is evaporated to dryness in vacuo, adding a small amount of water, and then ether to remove excess hydrochloric acid. After removing the excess HC1, the substance precipitates under ether. It is filtered off, and the filtrate is again evaporated in vacuo to dryness and an additional amount of the substance is obtained. The total yield of o-methyl urea hydrochloride is 4.7-5.7 g (40-50% or theoretical, calculated as urea).
Вычислено, %: С 21,69; И 6,38; N 25,35; Calculated,%: C 21.69; And 6.38; N 25.35;
0 НС1 33,00.0 HC1 33.00.
CaH ONaCl.CaH ONaCl.
Найдено, с 21,62; Н 6,49; N 25,18; НС1 33,03.Found with 21.62; H 6.49; N 25.18; HC1 33.03.
Содержание NIS составл ет 11,4 ат. % The NIS content is 11.4 atm. %
5 ( определено масс-спектрометрически).5 (determined by mass spectrometry).
Часть пикрата о-метилизомочевины перекристаллизовывают из гор чей воды; т. пл. вещества 192-194°С; пикрат о-метилизомочевины , получен из цианалида; т. пл. 194- A portion of the picrate of o-methylisourea is recrystallized from hot water; m.p. substances 192-194 ° C; o-methylisourea picrate, obtained from cyanalide; m.p. 194-
0 195°С; дл смещанной пробы т. пл. 192,5- 194°С.0 195 ° C; for the displaced sample t. pl. 192.5-194 ° C.
Предмет изобретени Subject invention
5 Способ получени меченой .о-метилизомочеQHHbi-N ,-. отличающийс тем, что меченую5 A method for the preparation of labeled. O-methyl isomer QHHbi-N, -. characterized in that labeled
мочевину-Н подвергают взаимодействию i диметилсульфатом при нагревании до 120°С.urea-H is subjected to the interaction of i dimethyl sulfate when heated to 120 ° C.
Publications (1)
| Publication Number | Publication Date |
|---|---|
| SU173746A1 true SU173746A1 (en) |
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