SU149430A1 - The method of obtaining 2,2,5-trimethoxy-2,5-dihydrofuran - Google Patents
The method of obtaining 2,2,5-trimethoxy-2,5-dihydrofuranInfo
- Publication number
- SU149430A1 SU149430A1 SU744128A SU744128A SU149430A1 SU 149430 A1 SU149430 A1 SU 149430A1 SU 744128 A SU744128 A SU 744128A SU 744128 A SU744128 A SU 744128A SU 149430 A1 SU149430 A1 SU 149430A1
- Authority
- SU
- USSR - Soviet Union
- Prior art keywords
- dihydrofuran
- trimethoxy
- obtaining
- bromofuran
- distilled
- Prior art date
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- Lubricants (AREA)
Description
Известны способы получени 2,2,5-триметокси-2,5-дигидрофурана по реакции электролитического метоксилировани производных фурана.Known methods for producing 2,2,5-trimethoxy-2,5-dihydrofuran by the reaction of electrolytic methoxylation of furan derivatives.
Предлагаемый способ отличаетс тем, что дл получени 2,2,5-триметокси-2 ,5-дигидрофурана используют 2-бромфуран.The proposed method is characterized in that 2-bromofuran is used to obtain 2,2,5-trimethoxy-2, 5-dihydrofuran.
При осуществлении способа электролизуют 2-бромфуран в смеси с метанолом и серной кислотой.When carrying out the process, 2-bromofuran is mixed with methanol and sulfuric acid.
Пример. В электролизер загружают 130 ж.л абсолютного метанола , 0,8 мл концентрированной M2SO4 и 5,9 г (0,04 мол ) 2-бромфурана. Электролизер представл ет собой стекл нный пробиркообразный цилиндр высотой 16 еж и диаметром 3,5 см. В качестве электродов используют угольные стержни диаметром 8 мм. Электролизер снабжен мешалкой и термометром и погружен в сосуд Дюара с бутиловым спиртом , охлаждаемым твердой углекислотой.Example. 130 liters of absolute methanol, 0.8 ml of concentrated M2SO4 and 5.9 g (0.04 mol) of 2-bromofuran are charged to the electrolyzer. The electrolyzer is a glass tube-shaped cylinder 16 hedgehogs high and 3.5 cm in diameter. Carbon rods with a diameter of 8 mm are used as electrodes. The electrolyzer is equipped with a stirrer and a thermometer and immersed in a Dewar vessel with butyl alcohol cooled by solid carbon dioxide.
Электролиз ведут посто нным током, плотностью на электроде от 2 до 4 , и температуре электролита - 15-20°. Сила тока - 0,9 а. По прекращению электролиза электролит нейтрализуют метилатом натри до . Метиловый спирт отгон ют, а к остатку добавл ют 50 мл сухого эфира. При этом выпадает сульфат натри , который отфильтровьшают, а эфир отгон ют. Остаток перегон ют при 190-200° (750 мм Hg). Получают 6,4 г светло-зеленой прозрачной жидкости (пп 1,4390), которую перегон ют в вакууме на елочном дефлегматоре высотой 10 см. При остаточном давлении 12 мм Hg собирают фракцию 82-85°. Выход - 4,6 г (72% от теоретического).The electrolysis is conducted with a direct current, a density of 2 to 4 on the electrode, and an electrolyte temperature of 15–20 °. Current - 0.9 a. Upon termination of the electrolysis, the electrolyte is neutralized with sodium methoxide. Methyl alcohol was distilled off, and 50 ml of dry ether was added to the residue. This releases sodium sulfate, which is filtered off and the ether is distilled off. The residue is distilled at 190-200 ° (750 mm Hg). 6.4 g of a light green transparent liquid (PP 1.4390) is obtained, which is distilled under vacuum on a Christmas tree reflux condenser 10 cm high. At a residual pressure of 12 mm Hg, a fraction of 82-85 ° is collected. The output is 4.6 g (72% of theoretical).
2,2,5-триметокси-2,5-дигидрофуран представл ет собой прозрачную масл нистую жидкость, не смешивающуюс с водой и большинством обычных органических растворителей.2,2,5-trimethoxy-2,5-dihydrofuran is a clear oily liquid that is immiscible with water and most common organic solvents.
№ 149430- 2 Свойства: . 1,4340; d - 1,0687.№ 149430- 2 Properties:. 1.4340; d - 1,0687.
Состав, %: С - 52,22; Н - 7.43 найдено) и С - 52,49; Н - 7,55 (вычислено дл C7Hi2O4).Composition,%: C - 52.22; H - 7.43 found) and C - 52.49; H - 7.55 (calculated for C7Hi2O4).
Предмет изобретени Subject invention
Способ получени 2,2,5-триметокси-2,5-дигидрофурана по реакции электролитического метоксилировани производных фурана, отличающийс тем,, что в качестве исходного берут 2-бромфуран,The method of obtaining 2,2,5-trimethoxy-2,5-dihydrofuran by the reaction of electrolytic methoxylation of furan derivatives, characterized in that 2-bromofuran is taken as the starting material,
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
SU744128A SU149430A1 (en) | 1961-09-08 | 1961-09-08 | The method of obtaining 2,2,5-trimethoxy-2,5-dihydrofuran |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
SU744128A SU149430A1 (en) | 1961-09-08 | 1961-09-08 | The method of obtaining 2,2,5-trimethoxy-2,5-dihydrofuran |
Publications (1)
Publication Number | Publication Date |
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SU149430A1 true SU149430A1 (en) | 1961-11-30 |
Family
ID=48304556
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
SU744128A SU149430A1 (en) | 1961-09-08 | 1961-09-08 | The method of obtaining 2,2,5-trimethoxy-2,5-dihydrofuran |
Country Status (1)
Country | Link |
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SU (1) | SU149430A1 (en) |
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1961
- 1961-09-08 SU SU744128A patent/SU149430A1/en active
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