SU520340A1 - The method of joint production of conjugated diolefins and sulfur-containing compounds - Google Patents
The method of joint production of conjugated diolefins and sulfur-containing compoundsInfo
- Publication number
- SU520340A1 SU520340A1 SU2051515A SU2051515A SU520340A1 SU 520340 A1 SU520340 A1 SU 520340A1 SU 2051515 A SU2051515 A SU 2051515A SU 2051515 A SU2051515 A SU 2051515A SU 520340 A1 SU520340 A1 SU 520340A1
- Authority
- SU
- USSR - Soviet Union
- Prior art keywords
- sulfur
- containing compounds
- conjugated diolefins
- joint production
- dioxane
- Prior art date
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Description
(2 моль) 4,4-диметил-1,3-ДИоксана, 540 г (моль) бутил меркаптана и 2 г серной кислоты, кип т т при j80°C, отбира по мере образоваш с верха j ректификационной колонки нзопрен с водой,| и пЬлучагот 111 г (80% в расчете на исходный диokcaM ) изопрена высокой степени чистоты, физккь-химические константы которого после сушки совпадают с литературными. 5,7-Дитиоувдеи н очи1Шют BaKWMHou дистилл цией, т.кип. 132-133°С/ /5 мм; п 1,5144; выход 84,9% ( в расчете на исходньш диоксан).(2 mol) 4,4-dimethyl-1,3-Dioxane, 540 g (mol) butyl mercaptan and 2 g of sulfuric acid, are boiled at j80 ° C, selected as from the top j of the distillation column nzoprene with water, | and a weight of 111 g (80% calculated on the starting dioxcaM) of high purity isoprene, the physical and chemical constants of which, after drying, coincide with the literature ones. 5,7-Dithio-wendeen niCh1Shut BaKWMHou by distillation, b.p. 132-133 ° C / / 5 mm; p 1,5144; yield 84.9% (based on the initial dioxane).
ИК-отектр, , 724-725 (сл.С-З-С), 2964 ( СН).IR, spectrum,, 724-725 (sl.S-Z-S), 2964 (CH).
Пример 2. 260 г (2 моль) 4,4,5-триметш1-1 ,3-ДИОксана,54Р г (6 моль) бутилмеркаптана и 60 г катеонита КУ-2 (СОЕ 4,95 мг-экв/г, влажность 30%) нагревают в , трехгорлой колбе,;Example 2. 260 g (2 mol) of 4,4,5-trimetsh1-1, 3-DIOxane, 54P g (6 mol) of butylmercaptan and 60 g of cathionite KU-2 (Eu of 4.95 mEq / g, humidity 30 %) heated in a three-neck flask;
снабженной ректификационной колонкой т.т25)| и механической мешалкой, при SO°C в течение S Час. С верха ректификационной колонки отбирают 2,3-диметилбутадиен-1,3. ВыхЪд 140 г (85% в расчете на исходный диоксан); т. кип. 68,5; 11 1,4378; d 0,7289.equipped with a distillation column tt25) | and mechanical stirrer, at SO ° C for S Hour. 2,3-dimethylbutadiene-1,3 is taken from the top of the distillation column. Output 140 g (85% calculated on the original dioxane); m.p. 68.5; 11 1.4378; d 0.7289.
Выход 5,7-дитиоундекана 87.4% (в расчете Ни исходный диоксан), физико-химические и спект палы«ые характеристики те же, что и в примере 1.The yield of 5,7-dithioundecane is 87.4% (in the calculation of neither the initial dioxane), the physicochemical and spectra of the characteristics are the same as in example 1.
Пример 3. 39 rf (0,3 моль) 4,4,5-триметилМ ,3-даоксана и 37,2 г (0,6 моль) зтилмеркаптана перемешивают 5 час при 150°С в металлической ампуле. При этом давление в системе дсстагает J5,8 атм. О конце реакции суд т по снижению давлени до 3 атм.Example 3. 39 rf (0.3 mol) of 4,4,5-trimethylM, 3-daoxane and 37.2 g (0.6 mol) of methyl mercaptan are mixed for 5 hours at 150 ° C in a metal ampoule. The pressure in the system dstagayet J5,8 atm. About the end of the reaction is judged by reducing the pressure to 3 atm.
Получают 20,9 г (85% на исходный диоксан) 2,3-диметил-1,3-бутадиена, т.кип. 68-69°С; П 1,4377; dj 0,7289, и 35,9 г (88% в расчете на исходньп диоксан) 3,5-ди1иогептана, т.кип. 72-74 С 18 мм; п1 1,50П.Get to 20.9 g (85% on the original dioxane) 2,3-dimethyl-1,3-butadiene, BP. 68-69 ° C; P 1.4377; dj 0.7289, and 35.9 g (88% based on the initial dioxane) of 3,5-di1ioheptane, b.p. 72-74 С 18 mm; P1 1.50P.
Claims (2)
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
SU2051515A SU520340A1 (en) | 1974-07-25 | 1974-07-25 | The method of joint production of conjugated diolefins and sulfur-containing compounds |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
SU2051515A SU520340A1 (en) | 1974-07-25 | 1974-07-25 | The method of joint production of conjugated diolefins and sulfur-containing compounds |
Publications (1)
Publication Number | Publication Date |
---|---|
SU520340A1 true SU520340A1 (en) | 1976-07-05 |
Family
ID=20593444
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
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SU2051515A SU520340A1 (en) | 1974-07-25 | 1974-07-25 | The method of joint production of conjugated diolefins and sulfur-containing compounds |
Country Status (1)
Country | Link |
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SU (1) | SU520340A1 (en) |
-
1974
- 1974-07-25 SU SU2051515A patent/SU520340A1/en active
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