SU197612A1 - METHOD OF OBTAINING 3,5-DINITRO-4-CHLORBENZOTRIFTORIDE - Google Patents
METHOD OF OBTAINING 3,5-DINITRO-4-CHLORBENZOTRIFTORIDEInfo
- Publication number
- SU197612A1 SU197612A1 SU1049873A SU1049873A SU197612A1 SU 197612 A1 SU197612 A1 SU 197612A1 SU 1049873 A SU1049873 A SU 1049873A SU 1049873 A SU1049873 A SU 1049873A SU 197612 A1 SU197612 A1 SU 197612A1
- Authority
- SU
- USSR - Soviet Union
- Prior art keywords
- dinitro
- obtaining
- chlorbenzotriftoride
- temperature
- chlorobenzotrifluoride
- Prior art date
Links
- 239000000203 mixture Substances 0.000 description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 230000000802 nitrating Effects 0.000 description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 4
- HFHAVERNVFNSHL-UHFFFAOYSA-N 2-chloro-1,3-dinitro-5-(trifluoromethyl)benzene Chemical compound [O-][N+](=O)C1=CC(C(F)(F)F)=CC([N+]([O-])=O)=C1Cl HFHAVERNVFNSHL-UHFFFAOYSA-N 0.000 description 3
- QULYNCCPRWKEMF-UHFFFAOYSA-N Parachlorobenzotrifluoride Chemical compound FC(F)(F)C1=CC=C(Cl)C=C1 QULYNCCPRWKEMF-UHFFFAOYSA-N 0.000 description 2
- DGRVQOKCSKDWIH-UHFFFAOYSA-N 1-chloro-2-(trifluoromethyl)benzene Chemical compound FC(F)(F)C1=CC=CC=C1Cl DGRVQOKCSKDWIH-UHFFFAOYSA-N 0.000 description 1
- TZGFQIXRVUHDLE-UHFFFAOYSA-N 1-chloro-2-nitro-4-(trifluoromethyl)benzene Chemical compound [O-][N+](=O)C1=CC(C(F)(F)F)=CC=C1Cl TZGFQIXRVUHDLE-UHFFFAOYSA-N 0.000 description 1
- GETTZEONDQJALK-UHFFFAOYSA-N Trifluorotoluene Chemical compound FC(F)(F)C1=CC=CC=C1 GETTZEONDQJALK-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Description
Известен способ получени 3,5-динитро-4хлорбензотрифторида путем обработки 3-нитро-4-хЛОрбензотрифторида нитрующей смесью, состо щей из азотной кислоты и 30Vo олеума.A known method for producing 3,5-dinitro-4chlorobenzotrifluoride by treating 3-nitro-4-chlorobenzotrifluoride with a nitrating mixture consisting of nitric acid and 30Vo oleum.
С целью увеличени выхода 3,5-динитро-4хлорбензотрифторида , а также повышени степени чистоты его, предложен способ, но которому 4-хлорбензотрифторид обрабатывают нитрующей смесью, состо щей из азотной кислоты и 170/0 олеума.In order to increase the yield of 3,5-dinitro-4chlorobenzotrifluoride, as well as to increase its purity, a method has been proposed, but in which 4-chlorobenzotrifluoride is treated with a nitrating mixture consisting of nitric acid and 170/0 oleum.
Пример. В реактор, снабженный механической мешалкой, термометром, обратным холодильником и капельной воронкой, помещают 120 мл 170/о-ного олеума и при размешивании и охлаждении прибавл ют 50 мл азотной кислоты (уд. в. 1,52), поддержива температуру не выше 40° С. К полученной 1нтрующей смеси в течение 0,5 час при температуре 40-50° С добавл ют 20 г -хлорбензотрифторида при интенсивном перемещивании, после чего массу нагревают в течение 0,5 час до температуры 105-107° С и размещивают при этой температуре 0,5 час. Затем температуру повышают до 120-125° С и перемешивают при этой температуре 15 мин. Далее содерл имое реактора охлаждают при комнатной температуре п выливают на лед. Осадок отфильтровывают, промывают водой от кислот и сушат. Выход 27,4 г (9lVo), т. пл. 55-56° С. Аналитически чистый образец имеет т. нл. 47-58° С.Example. In a reactor equipped with a mechanical stirrer, a thermometer, a reflux condenser and a dropping funnel, 120 ml of 170 / o-oleum are placed and, while stirring and cooling, 50 ml of nitric acid (sp. ° C. To the obtained 1NT mixture, for 0.5 hour at a temperature of 40-50 ° C, add 20 g of chlorobenzotrifluoride with intensive movement, after which the mass is heated for 0.5 hour to a temperature of 105-107 ° C and placed at this temperature 0.5 hours. Then the temperature is raised to 120-125 ° C and stirred at this temperature for 15 minutes. Next, the contents of the reactor are cooled at room temperature and poured onto ice. The precipitate is filtered off, washed with water from acids and dried. The yield of 27.4 g (9lVo), so pl. 55-56 ° C. The analytically pure sample has t. Nl. 47-58 ° C.
Предмет изобретени Subject invention
Способ получени 3,5-динитро-4-хлорбензотрифторида путем обработки производныхThe method of obtaining 3,5-dinitro-4-chlorobenzotrifluoride by treating derivatives
бензотрифторида нитрующей смесью, состо щей пз азотной кислоты и олеума, отличающийс тем, что, с целью увеличени выхода целевого продукта и его чистоты, в качестве производного бензотрнфторида берут 4-хлорбензотрифторид и обрабатывают последний нитрующей смесью, содержащей 17а/о олеума.benzotrifluoride with nitrating mixture consisting of nitric acid and oleum, characterized in that, in order to increase the yield of the target product and its purity, 4-chlorobenzotrifluoride is taken as benzotrnfluoride derivative and treated with the latter with a nitrating mixture containing 17a / o oleum.
Publications (1)
| Publication Number | Publication Date |
|---|---|
| SU197612A1 true SU197612A1 (en) |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4096195A (en) * | 1977-05-13 | 1978-06-20 | Gaf Corporation | Cyclic two-stage nitration process for preparing 4-chloro-3,5-dinitrobenzotrifluoride from 4-chlorobenzotrifluoride |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4096195A (en) * | 1977-05-13 | 1978-06-20 | Gaf Corporation | Cyclic two-stage nitration process for preparing 4-chloro-3,5-dinitrobenzotrifluoride from 4-chlorobenzotrifluoride |
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