SU255285A1 - - Google Patents
Info
- Publication number
- SU255285A1 SU255285A1 SU1273837A SU1273837A SU255285A1 SU 255285 A1 SU255285 A1 SU 255285A1 SU 1273837 A SU1273837 A SU 1273837A SU 1273837 A SU1273837 A SU 1273837A SU 255285 A1 SU255285 A1 SU 255285A1
- Authority
- SU
- USSR - Soviet Union
- Prior art keywords
- tripyryl
- pyrrolkali
- triazine
- tetrahydrofuran
- pyrrole
- Prior art date
Links
- WYURNTSHIVDZCO-UHFFFAOYSA-N tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 8
- 229910052783 alkali metal Inorganic materials 0.000 claims description 2
- -1 alkali metal salt Chemical class 0.000 claims description 2
- 239000003960 organic solvent Substances 0.000 claims description 2
- KAESVJOAVNADME-UHFFFAOYSA-N pyrrole Chemical compound C=1C=CNC=1 KAESVJOAVNADME-UHFFFAOYSA-N 0.000 claims description 2
- 239000011780 sodium chloride Substances 0.000 claims description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims 1
- 238000002955 isolation Methods 0.000 claims 1
- 238000000034 method Methods 0.000 claims 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- MGNCLNQXLYJVJD-UHFFFAOYSA-N Cyanuric chloride Chemical compound ClC1=NC(Cl)=NC(Cl)=N1 MGNCLNQXLYJVJD-UHFFFAOYSA-N 0.000 description 2
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 2
- CSCPPACGZOOCGX-UHFFFAOYSA-N acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- ZFSLODLOARCGLH-UHFFFAOYSA-N Cyanuric acid Chemical compound OC1=NC(O)=NC(O)=N1 ZFSLODLOARCGLH-UHFFFAOYSA-N 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- XTLNYNMNUCLWEZ-UHFFFAOYSA-N ethanol;propan-2-one Chemical compound CCO.CC(C)=O XTLNYNMNUCLWEZ-UHFFFAOYSA-N 0.000 description 1
- 239000000543 intermediate Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 238000005020 pharmaceutical industry Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000002194 synthesizing Effects 0.000 description 1
Description
Изобретение относитс к области получени новой системы соединений, которые могут найти применение в фармацевтической промышленности в качестве полупродуктов дл синтеза красителей.The invention relates to the field of obtaining a new system of compounds that can be used in the pharmaceutical industry as intermediates for the synthesis of dyes.
Предлагаемый способ получени 2,4,6-трипиррил-5-триазина заключаетс в том, что цианурхло ид подвергают взаимодействию с солью щелочного металла пиррола, например пирролкалием, в среде органического растворител , например тетрагидрофурана, преимуществ енно при температуре 15-25°С. Продукты выдел ют известным способом. Выход около 620/0Пример . К раствору 26,2 г (0,250 лоль) пирролкали в 100 мл тетрагидрофурана, помещенному в колбу с обратным холодильником , мешалкой и термометром, при 15-25°С приливают раствор 15 г цианурхлорида в 150 мл, тетрагидрофурана.The proposed method for the preparation of 2,4,6-tripyryl-5-triazine is that the cyanuric acid is reacted with an alkali metal salt of pyrrole, for example pyrrolkali, in an organic solvent medium, for example tetrahydrofuran, preferably at a temperature of 15-25 ° C. Products are isolated in a known manner. Output about 620/0 Example. To a solution of 26.2 g (0.250 L) of pyrrolkali in 100 ml of tetrahydrofuran, placed in a flask with reflux condenser, a stirrer and a thermometer, a solution of 15 g of cyanuric chloride in 150 ml of tetrahydrofuran is poured at 15-25 ° C.
Конденсацию провод т при 15-25°С в токе азота при хорошем перемешивании в течение 18 час.The condensation is carried out at 15-25 ° C in a stream of nitrogen with good stirring for 18 hours.
После выдержки смесь выливают в воду. Выпавший продукт отфильтровывают, хорошо промывают водой и сушат.After aging the mixture is poured into water. The precipitated product is filtered off, washed well with water and dried.
После перекристаллизации из смеси ацетон - этанол {80 : 20) выход продукта 13,9 г, т. е. 62% от цианурхлорида.After recrystallization from a mixture of acetone - ethanol {80: 20), the product yield is 13.9 g, i.e. 62% of cyanuric chloride.
Полученный 2,4,6-трипиррил-5-триазин с т. пл. 183°С представл ет собой белые игольчатые кристаллы. Хорошо раствор етс в ацетоне , диметилформамиде, плохо - в этаноле и «е раствор етс в воде.The resulting 2,4,6-tripyryl-5-triazine with m. Pl. 183 ° C are white needles. It dissolves well in acetone, dimethylformamide, poorly in ethanol and is not soluble in water.
Найдено, %: С 65,8, 65,47; В 4,29, 4,18; N 30,31, 30,24.Found,%: C 65.8, 65.47; B 4.29, 4.18; N 30.31, 30.24.
Вычислено, о/„: С 65„3; Н 4,3; N 30,4.Calculated, о / „: С 65„ 3; H 4.3; N 30.4.
CisHiaNo.CisHiaNo.
Предмет изО|бретени Subject of use
Claims (2)
Publications (1)
Publication Number | Publication Date |
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SU255285A1 true SU255285A1 (en) |
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