SU149430A1 - The method of obtaining 2,2,5-trimethoxy-2,5-dihydrofuran - Google Patents

The method of obtaining 2,2,5-trimethoxy-2,5-dihydrofuran

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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
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SU
USSR - Soviet Union
Prior art keywords
dihydrofuran
trimethoxy
obtaining
bromofuran
distilled
Prior art date
Application number
SU744128A
Other languages
Russian (ru)
Inventor
С.А. Гиллер
Г.П. Соколов
Original Assignee
С.А. Гиллер
Г.П. Соколов
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
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Publication date
Application filed by С.А. Гиллер, Г.П. Соколов filed Critical С.А. Гиллер
Priority to SU744128A priority Critical patent/SU149430A1/en
Application granted granted Critical
Publication of SU149430A1 publication Critical patent/SU149430A1/en

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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,

SU744128A 1961-09-08 1961-09-08 The method of obtaining 2,2,5-trimethoxy-2,5-dihydrofuran SU149430A1 (en)

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
SU149430A1 true SU149430A1 (en) 1961-11-30

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