SU134265A1 - The method of obtaining quinuclidon-3 - Google Patents
The method of obtaining quinuclidon-3Info
- Publication number
- SU134265A1 SU134265A1 SU658863A SU658863A SU134265A1 SU 134265 A1 SU134265 A1 SU 134265A1 SU 658863 A SU658863 A SU 658863A SU 658863 A SU658863 A SU 658863A SU 134265 A1 SU134265 A1 SU 134265A1
- Authority
- SU
- USSR - Soviet Union
- Prior art keywords
- quinuclidon
- obtaining
- carbethoxypiperidine
- quinuclidone
- carbethoxymethyl
- Prior art date
Links
Landscapes
- Nitrogen Condensed Heterocyclic Rings (AREA)
Description
В качестве конденсирующего средства используют металлический калий или этилат «али . Выход хинуклидона-3 (III), счита на диэфир (I) составл ет в первом случае 37-44%, во втором 68-70% от теоретического .Metallic potassium or ethylate ali is used as a condensing agent. The yield of quinuclidone-3 (III), calculated as diester (I), is 37-44% in the first case, 68-70% of the theoretical in the second.
Предложенный способ получени хинуклидона-3 отличаетс тем, что реакцию конденсации 1-карбэтоксиметил-4-карб9токсипиперидина провод т при нагревании в присутствии н-бутилата кали , получаемого известными приемами из н-бутилового спирта и едкого кали. Способ более прост и огневзрывобезопасен.The proposed method for the preparation of quinuclidone-3 is characterized in that the condensation reaction of 1-carbethoxymethyl-4-carb9-toxy-piperidine is carried out by heating in the presence of potassium n-butylate, produced by known methods from n-butyl alcohol and potassium hydroxide. The method is more simple and fireproof.
Пример. В 2-литровую колбу, снабженную мещалкой, обратным холодильником и насадкой Дина и Старка, помещают 69,2 г едкою кали.Example. In a 2-liter flask equipped with a broom, a reflux condenser, and a Dean and Stark nozzle, 69.2 g of potassium hydroxide are placed.
.Nb 3126П.Nb 3126P
1000 мл н-бутилового спирта и 100 мл толуола. Смесь кип т т до прекращени отделени воды, затем упаривают в вакууме (при 15-20 мм) досуха, довод температуру масл ной бани под конец отгонки до 200°.1000 ml of n-butyl alcohol and 100 ml of toluene. The mixture is boiled until the separation of water ceases, then it is evaporated in vacuo (at 15-20 mm) to dryness, bringing the oil bath temperature to 200 ° at the end of distillation.
К твердому остатку прибавл ют 200 мл безводного толуола, смесь нагревают до кипени и затем при перемешивании приливают в течение часа раствор 120 г 1-карбэтоксиметил-4-карбэтоксипиперидиай.и 300 мл толуола. Реакционную массу кип т т в течение п ти часов, охлаждают до 20 и обрабатывают 400 мл концентрированной сол ной кислотой:.200 ml of anhydrous toluene was added to the solid residue, the mixture was heated to boiling, and then a solution of 120 g of 1-carbethoxymethyl-4-carbethoxypiperidiynium and 300 ml of toluene was added with stirring over an hour. The reaction mass is boiled for five hours, cooled to 20 and treated with 400 ml of concentrated hydrochloric acid :.
Выделившийс хлористый кальций отфильтровывают, сол нокислый слой отдел ют от толуольпого, последний дважды экстрагируют 400 мл сол ной кислоты. Объединенные сол нокислые растворы кип т т 6 часов и упаривают. Остаток смешивают при охлаждении с 140 мл 50%-ного раствора едкого кали и продукт из ш;елочного раствора экстрагируют бензолом. После отгонки бензола 43,4 г хинуклидона-3 с т. пл. 133-135°. Т. пл. пикрата 210°. Выход 70% от теоретического .The precipitated calcium chloride is filtered off, the hydrochloric acid layer is separated from the toluene layer, the latter is extracted twice with 400 ml of hydrochloric acid. The combined hydrochloric acid solutions are boiled for 6 hours and evaporated. The residue is mixed while cooling with 140 ml of a 50% strength solution of potassium hydroxide and the product is extracted from benzene solution and benzene. After distilling off benzene, 43.4 g of quinuclidone-3 with m. Pl. 133-135 °. T. pl. picrate 210 °. Yield 70% of theoretical.
Предмет изобпетени Subject matter
Способ получени хинуклидона-3 из 1-карбэтоксиметил-4Карбэтоксипиперидина , отличающийс тем, что, с целью уменьшени огневзрывоопасности производства, реакцию конденсации 1-карбэтоксиметил-4-карбэтоксипиперидина провод т нагреваниеив присутствии н-бутилата кали , получаемого известными приемами из н-бутилового спирта и едкого кали..The method of producing quinuclidone-3 from 1-carbethoxymethyl-4-Carbethoxypiperidine, characterized in that, in order to reduce production fire hazard, the condensation reaction of 1-carbethoxymethyl-4-carbethoxypiperidine is heated in the presence of potassium n-butylate produced by means of izdplains, I, I, I, I, I, I, I, I, I, I, I, I, you can use the settings for the production of i-carbethoxypiperidine-3-carbethoxypiperidine caustic potash ..
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
SU658863A SU134265A1 (en) | 1960-03-16 | 1960-03-16 | The method of obtaining quinuclidon-3 |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
SU658863A SU134265A1 (en) | 1960-03-16 | 1960-03-16 | The method of obtaining quinuclidon-3 |
Publications (1)
Publication Number | Publication Date |
---|---|
SU134265A1 true SU134265A1 (en) | 1960-11-30 |
Family
ID=48405235
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
SU658863A SU134265A1 (en) | 1960-03-16 | 1960-03-16 | The method of obtaining quinuclidon-3 |
Country Status (1)
Country | Link |
---|---|
SU (1) | SU134265A1 (en) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3342828A (en) * | 1967-09-19 | Method of producing |
-
1960
- 1960-03-16 SU SU658863A patent/SU134265A1/en active
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3342828A (en) * | 1967-09-19 | Method of producing |
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