SU174630A1 - METHOD FOR OBTAINING A THIOSEMICARBAZON OR SELICICARBAZON BARBITURIC ACID - Google Patents
METHOD FOR OBTAINING A THIOSEMICARBAZON OR SELICICARBAZON BARBITURIC ACIDInfo
- Publication number
- SU174630A1 SU174630A1 SU907550A SU907550A SU174630A1 SU 174630 A1 SU174630 A1 SU 174630A1 SU 907550 A SU907550 A SU 907550A SU 907550 A SU907550 A SU 907550A SU 174630 A1 SU174630 A1 SU 174630A1
- Authority
- SU
- USSR - Soviet Union
- Prior art keywords
- barbituric acid
- thiosemicarbazon
- selicicarbazon
- obtaining
- solution
- Prior art date
Links
- HNYOPLTXPVRDBG-UHFFFAOYSA-N Barbituric acid Chemical compound O=C1CC(=O)NC(=O)N1 HNYOPLTXPVRDBG-UHFFFAOYSA-N 0.000 title description 7
- 239000000243 solution Substances 0.000 description 4
- SRVJKTDHMYAMHA-WUXMJOGZSA-N Thioacetazone Chemical compound CC(=O)NC1=CC=C(\C=N\NC(N)=S)C=C1 SRVJKTDHMYAMHA-WUXMJOGZSA-N 0.000 description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-N acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- SCVFZCLFOSHCOH-UHFFFAOYSA-M Potassium acetate Chemical compound [K+].CC([O-])=O SCVFZCLFOSHCOH-UHFFFAOYSA-M 0.000 description 2
- BRWIZMBXBAOCCF-UHFFFAOYSA-N aminothiourea Chemical compound NNC(N)=S BRWIZMBXBAOCCF-UHFFFAOYSA-N 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 235000019441 ethanol Nutrition 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000011541 reaction mixture Substances 0.000 description 2
- 150000007659 semicarbazones Chemical class 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- DUIOPKIIICUYRZ-UHFFFAOYSA-N Semicarbazide Chemical compound NNC(N)=O DUIOPKIIICUYRZ-UHFFFAOYSA-N 0.000 description 1
- XHQYBDSXTDXSHY-UHFFFAOYSA-N Semicarbazide hydrochloride Chemical compound Cl.NNC(N)=O XHQYBDSXTDXSHY-UHFFFAOYSA-N 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- -1 barbituric acid semicarbazone Chemical compound 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 235000011056 potassium acetate Nutrition 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 239000012047 saturated solution Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Description
Предложен способ получени тиосемикарбазона или семикарбазона барбитуровой кислоты , заключающийс во взаимодействии барбитуровой кислоты с тпосемижарбазидом или с семикарбазидом соответствепно. Выход целевых продуктов 50-60%.A method for the preparation of thiosemicarbazone or semicarbazone of barbituric acid is proposed. The yield of the target products 50-60%.
Полученные соединени в литературе не олисаны, они могут служить исходными продуктами дл получени ценных физиологически активных соединений.The compounds obtained in the literature are not olisanes; they can serve as starting materials for the preparation of valuable physiologically active compounds.
Пример 1. К раствору 0,1 моль барбитуровой КИСЛОТЫ в 250 мл 70%-ного этанола приливают раствор 0,1 моль тиосемикарбазида 3 150 мл этилового спирта. С.месь кип т т в Колбе с обратным холодильни-ком в течение 4 час.Example 1. To a solution of 0.1 mol of barbituric acid in 250 ml of 70% ethanol, a solution of 0.1 mol of thiosemicarbazide 3 is poured with 150 ml of ethyl alcohol. C. The mixture is boiled in a flask with a reflux condenser for 4 hours.
После охлаждени реакционной смеси осадок отфильтровывают и промывают водой. Выход 50-60%. После перекристаллизации получают тиосемикарбазон барбитуровой кислоты в виде бесцветного кристаллического вещества с температурой разложени выше 300°С.After cooling the reaction mixture, the precipitate is filtered and washed with water. Yield 50-60%. After recrystallization, thiosemicarbazone barbituric acid is obtained as a colorless crystalline substance with a decomposition temperature above 300 ° C.
Пример 2. К водному раствору 0,1 моль сол нокислого семикарбазида приливают раствор 0,1 моль барбитуровой кислоты в 50%ной уксусной кислоте. Реакционную смесь кип т т в КОлбе с обратным холодильником в течение 2 час. К остывшему раствору прибавл ют насыщенный раствор уксуснокислого кали . Выпавший осадок отфильтровывают, промывают водой и высушивают при колшатной температуре. Выход 48-50%. Полученный семикарбазон барбитуровой кислоты начинает разлагатьс .при нагревании свыше 215°С.Example 2. A solution of 0.1 mol of barbituric acid in 50% acetic acid is added to an aqueous solution of 0.1 mol of semicarbazide hydrochloride. The reaction mixture is refluxed for 2 hours. A saturated solution of potassium acetate is added to the cooled solution. The precipitation is filtered off, washed with water and dried at a pitched temperature. The yield is 48-50%. The barbituric acid semicarbazone obtained begins to decompose when heated above 215 ° C.
Предмет и з о б р е т е ,н in Subject and issue of n, in
Способ получени тиосемикарбазона или семикарбазона барбитуровой .кислоты, отличающийс тем, что барбитуровую кислоту подвергают взаимодействию с тиосеми-карбазидом или семикарбазидом при кип чении.A method for producing thiosemicarbazone or semicarbazone barbituric acid, characterized in that the barbituric acid is reacted with thiosemi-carbazide or semicarbazide at boiling.
Publications (1)
| Publication Number | Publication Date |
|---|---|
| SU174630A1 true SU174630A1 (en) |
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