SU234406A1 - METHOD OF OBTAINING 3-METHYL-ZN-IL / IDAZOLON-2- - Google Patents
METHOD OF OBTAINING 3-METHYL-ZN-IL / IDAZOLON-2-Info
- Publication number
- SU234406A1 SU234406A1 SU1148225A SU1148225A SU234406A1 SU 234406 A1 SU234406 A1 SU 234406A1 SU 1148225 A SU1148225 A SU 1148225A SU 1148225 A SU1148225 A SU 1148225A SU 234406 A1 SU234406 A1 SU 234406A1
- Authority
- SU
- USSR - Soviet Union
- Prior art keywords
- methyl
- idazolon
- obtaining
- urea
- cold
- Prior art date
Links
- XSQUKJJJFZCRTK-UHFFFAOYSA-N urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 6
- 239000004202 carbamide Substances 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N HCl Chemical compound Cl VEXZGXHMUGYJMC-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
- 238000000034 method Methods 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- OIGNJSKKLXVSLS-VWUMJDOOSA-N Prednisolone Chemical compound O=C1C=C[C@]2(C)[C@H]3[C@@H](O)C[C@](C)([C@@](CC4)(O)C(=O)CO)[C@@H]4[C@@H]3CCC2=C1 OIGNJSKKLXVSLS-VWUMJDOOSA-N 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 description 1
- WKBOTKDWSSQWDR-UHFFFAOYSA-N bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- JUJWROOIHBZHMG-UHFFFAOYSA-N pyridine Substances C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 1
- 239000011541 reaction mixture Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Description
Изобретение относитс к области получени производных нмпдазолонов, прнмен емых в органическом синтезе.The invention relates to the field of the preparation of nmpdazolone derivatives, applied in organic synthesis.
Известный снособ получени ЗИ-нмидазолон-2 (4,5-6)-иириднна заключайс в том, что метанольныи раствор 2-аминоникот11намида кии т т с воднощелочнллм раствором брома .The well-known ZI-nmidazolon-2 (4,5-6) -iird preparation method consists in the fact that a methanolic solution of 2-aminonicotone is hydrated with water-alkaline solution of bromine.
С целью хпрощеии те.хнологнческого процесса , предлагаетс получать 3-метнл-ЗН-имидазолон-2- (4,S-i)-пиридин сплавленпем сол нокнслого 2-метила.мнно-З-аминопнридина с мочевиной прн 160-180С с носледуюпднм выделением целевого продукта нзвестньп способом.In order to achieve a better technological process, it is proposed to obtain 3-methyl-3H-imidazolone-2- (4, Si) -pyridine fused solone layer of 2-methyl m-3-aminophenridine with urea prn 160-180C with the next generation of the desired product well-known way.
Пример. Сменишают в тигле 1,5 г мочевины и 1,5 г сол нокислого 2-метиламино-Замннопирнднна , плав т содержимое тигл , нагревают до 160-1 80 С и выдерживают примерно 15 мин при этой температуре. Затвердевшую реакционную массу охлаждают, измельчают в воде ( мл), кип т т 3-5 мин, отфильтровывают полученный сероватый порошок , промывают его холодной водой, небольншм количеством холодного сппрта, затем эфиром н сушат. Выход продукта 50%, т. пл. 234-235°С (после перекристаллнзацин этанола).Example. The crucible is replaced with 1.5 g of urea and 1.5 g of 2-methylamino-Znamnirpirnn hydrochloric acid, the contents of the crucible are melted, heated to 160-180 ° C and kept for about 15 minutes at this temperature. The solidified reaction mixture is cooled, crushed in water (ml), boiled for 3-5 minutes, the resulting grayish powder is filtered off, washed with cold water, a small amount of cold cold, then ether n is dried. The product yield is 50%, so pl. 234-235 ° C (after recrystallized ethanol).
Пайдено. %: С 55,89: 56,08; П 4,77; 4,79; X 27,99; 28,12.Paydeno. %: C 55.89: 56.08; P 4.77; 4.79; X 27.99; 28.12.
Выч1тслено, %; С 56,36; П 4,73; N 28,17.Calculated%; C 56.36; P 4.73; N 28.17.
Предмет изобретени Subject invention
Снособ получени З-метнл-ЗП-имидазолон2- (4,5 /;)-ниридина, отличающийс тем, что, е целью унрош,ени технологического процесса, сел П окислы и 2-метнламино-3-амннопнрнд1И1 сплавл ют с мочевнной при 160-180 С с носледующнм выделением целевого продукта известным способом.The method for producing 3-methyl-3P-imidazolone-2 (4,5 /;) -neridine, characterized in that, for the purpose of the technological process, villages P oxides and 2-metnlamino-3 amnnrind1I1 are fused with urea at 160 -180 С with the following selection of the target product in a known manner.
Publications (1)
Publication Number | Publication Date |
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SU234406A1 true SU234406A1 (en) |
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