SU495314A1 - The method of obtaining dithienyls - Google Patents
The method of obtaining dithienylsInfo
- Publication number
- SU495314A1 SU495314A1 SU2051648A SU2051648A SU495314A1 SU 495314 A1 SU495314 A1 SU 495314A1 SU 2051648 A SU2051648 A SU 2051648A SU 2051648 A SU2051648 A SU 2051648A SU 495314 A1 SU495314 A1 SU 495314A1
- Authority
- SU
- USSR - Soviet Union
- Prior art keywords
- dithienyls
- obtaining
- mixture
- thiophene
- dithienyl
- Prior art date
Links
Landscapes
- Heterocyclic Carbon Compounds Containing A Hetero Ring Having Oxygen Or Sulfur (AREA)
Description
Пример 1. 20,0 г (0,24 моль) тиофена нагревают в кубе рециркул ционной установки до кицени и образующиес пары подаютс током сероводорода (2-3 л/час), затем в пустую кварцевую трубку длиной 520 мм и диаметром 30 мм, нагреваемую до 750°. Часть паров, попада далее в холодильник, конденсируетс и затем возвращаетс вновь дл подогрева. Процесс продолжаетс в течение 6 ч до прекращени поступлени паров исходного тиофена в реакционную зону, температура в кубе при этом повышаетс с 84 до 200°С. Перегонкой реакционной смеси получают 16,5 г (82,5%) смеси изомерных дитиенилов .Example 1. 20.0 g (0.24 mol) of thiophene is heated in a cube of the recirculation unit to Kietzee and the resulting vapors are fed with a current of hydrogen sulfide (2-3 l / h), then into an empty quartz tube 520 mm long and 30 mm in diameter, heated to 750 °. A portion of the vapor, which then goes further into the refrigerator, condenses and then returns again for heating. The process continues for 6 hours until the vapor of the starting thiophene enters the reaction zone, the temperature in the bottom rises from 84 to 200 ° C. Distillation of the reaction mixture yields 16.5 g (82.5%) of a mixture of isomeric dithienyls.
После разделени смеси изомерных дитиенилов на препаративном хроматографе (жидка фаза SE-30, 5%, носить хезасррб, температура колонки 150°, газ-носитель - гелий) получают а, а-дитиенил с т. пл. 32°С; а, рдитненил с т. пл. 63°С, и |3, (З-дитиенил с т. пл. 128°:С.After separation of the mixture of isomeric dithienyls on a preparative chromatograph (liquid phase SE-30, 5%, wearing hezasrb, column temperature 150 °, carrier gas — helium), a and a-dithienyl are obtained with m. Pl. 32 ° C; a, rditenil with t. pl. 63 ° С, and | 3, (S-ditien with mp 128 ° C).
Соотношение изомеров в смеси, % : а,а: а,- : |3, : 6 : 3.The ratio of isomers in the mixture,%: a, a: a, -: | 3,: 6: 3.
В масс-спектре смеси изомеров содержитс поглощающий гаик с 166.The mass spectrum of the mixture of isomers contains an absorbing nut with 166.
Найдено, %: С 58,35; Н 3,31; S 38,34.Found,%: C 58.35; H 3.31; S 38,34.
CgHgSs.CgHgSs.
Вычислено, %: С 58,03; Н 3,25; S 38,73.Calculated,%: C 58.03; H 3.25; S 38.73.
В ИК-спектрах а, а-дитиенила найдена полоса 700 см-1, а, р-дитиенила 778 см-, |3, рдитиенила 773 см.In the IR spectra of a, a-dithienyl, a 700 cm-1 band was found, a, p-dithienyl band was 778 cm-, | 3, rdithienyl was 773 cm.
Claims (1)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| SU2051648A SU495314A1 (en) | 1974-08-06 | 1974-08-06 | The method of obtaining dithienyls |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| SU2051648A SU495314A1 (en) | 1974-08-06 | 1974-08-06 | The method of obtaining dithienyls |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| SU495314A1 true SU495314A1 (en) | 1975-12-15 |
Family
ID=20593496
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| SU2051648A SU495314A1 (en) | 1974-08-06 | 1974-08-06 | The method of obtaining dithienyls |
Country Status (1)
| Country | Link |
|---|---|
| SU (1) | SU495314A1 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5158598A (en) * | 1988-08-04 | 1992-10-27 | Basf Aktiengesellschaft | Bithienyl derivatives, and herbicidal use for agents containing them |
-
1974
- 1974-08-06 SU SU2051648A patent/SU495314A1/en active
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5158598A (en) * | 1988-08-04 | 1992-10-27 | Basf Aktiengesellschaft | Bithienyl derivatives, and herbicidal use for agents containing them |
| EP0353667B1 (en) * | 1988-08-04 | 1994-03-16 | BASF Aktiengesellschaft | Bithienyl derivatives, process for their preparation, and compositions containing them |
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