SU3264A1 - The method of preparation of hydrochloric diacetylmorphine - Google Patents
The method of preparation of hydrochloric diacetylmorphineInfo
- Publication number
- SU3264A1 SU3264A1 SU811A SU811A SU3264A1 SU 3264 A1 SU3264 A1 SU 3264A1 SU 811 A SU811 A SU 811A SU 811 A SU811 A SU 811A SU 3264 A1 SU3264 A1 SU 3264A1
- Authority
- SU
- USSR - Soviet Union
- Prior art keywords
- hydrochloric
- preparation
- diacetylmorphine
- salt
- solution
- Prior art date
Links
- GVGLGOZIDCSQPN-PVHGPHFFSA-N Heroin Chemical compound O([C@H]1[C@H](C=C[C@H]23)OC(C)=O)C4=C5[C@@]12CCN(C)[C@@H]3CC5=CC=C4OC(C)=O GVGLGOZIDCSQPN-PVHGPHFFSA-N 0.000 title description 6
- 229960002069 diamorphine Drugs 0.000 title description 6
- 238000002360 preparation method Methods 0.000 title description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N HCl Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 9
- XEKOWRVHYACXOJ-UHFFFAOYSA-N acetic acid ethyl ester Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 5
- 150000003839 salts Chemical class 0.000 description 5
- 239000011780 sodium chloride Substances 0.000 description 5
- 235000019439 ethyl acetate Nutrition 0.000 description 4
- RTZKZFJDLAIYFH-UHFFFAOYSA-N diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 3
- 238000005755 formation reaction Methods 0.000 description 3
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 3
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 3
- JJGYGPZNTOPXGV-SSTWWWIQSA-N 6-Acetylmorphine Chemical compound O([C@H]1[C@H](C=C[C@H]23)OC(C)=O)C4=C5[C@@]12CCN(C)[C@@H]3CC5=CC=C4O JJGYGPZNTOPXGV-SSTWWWIQSA-N 0.000 description 2
- 229940120060 Heroin Drugs 0.000 description 2
- UHOVQNZJYSORNB-UHFFFAOYSA-N benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 230000008929 regeneration Effects 0.000 description 2
- 238000011069 regeneration method Methods 0.000 description 2
- 238000007792 addition Methods 0.000 description 1
- 239000005456 alcohol based solvent Substances 0.000 description 1
- UXVMQQNJUSDDNG-UHFFFAOYSA-L cacl2 Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 1
- 239000001110 calcium chloride Substances 0.000 description 1
- 229910001628 calcium chloride Inorganic materials 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000004210 ether based solvent Substances 0.000 description 1
- 150000003840 hydrochlorides Chemical class 0.000 description 1
- 239000012452 mother liquor Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000003247 radioactive fallout Substances 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 238000007127 saponification reaction Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Description
По -известному способу получени хлористоводородного диацетил-морфина (героина) основание раствор етс в органических растворител х, как, например , спирт или бензол, и к раствору прибавл ют необходимое количество хлористого водорода, а затем выдел ют хлоргидрат прибавлением серного эфира.In the well-known method of producing hydrochloric diacetyl-morphine (heroin), the base is dissolved in organic solvents, such as alcohol or benzene, and the required amount of hydrogen chloride is added to the solution, and then the hydrochloride is isolated by the addition of sulfuric ether.
Получение хлоргидрата по этому способу имеет следующие недостатки: соль неполностью выпадает в виде смолообразной массы, котора через некоторое врем закристаллизовываетс ; исходное основание должно быть безусловно чистое и не давать окрашенного раствора, иначе окраска увлекаетс 1выпадающей смолообразной Л1ассой и соль получаетс окрашенной; регенераци растворителей спирта и эфира затруднительна;необходимоупотребл ть абсолютный спирт и эфир, и происходит частичное омыление-образование моноацетил-морфина, в особенности при сгущении маточных растворов.The preparation of hydrochloride by this method has the following disadvantages: the salt does not fully fall out in the form of a resinous mass, which crystallizes over time; the original base must be unconditionally pure and not give a colored solution, otherwise the color is entrained by the falling resinous resin and the salt is colored; regeneration of alcohol and ether solvents is difficult; absolute alcohol and ether must be used, and partial saponification-formation of monoacetyl-morphine occurs, especially when the mother liquors are thickened.
По предлагаемому же способу средою , в которой идет солеобразование, беретс сухой уксусный эфир, а хлористый водород прибавл етс в виде крепкого (концентрированного) раствора в абсолютном спирту.According to the proposed method, dry acetic ether is added to the medium in which the salt formation occurs, and hydrogen chloride is added as a strong (concentrated) solution in absolute alcohol.
Хлористоводородна соль выпадает сразу в хорошем кристаллическом виде; соль получаетс совершенно белой и из окрашенных растворов, так что нет надобности исходить из совершенно чистого основани ; регенераци растворител - уксусного этилового эфира не представл ет никаких затруднений (сушка хлористым кальцием ) и по сгущении маточных растворов не получаетс продуктов омылени -моноацетил-морфина .The hydrochloride salt precipitates immediately in good crystalline form; salt is obtained completely white and from colored solutions, so that there is no need to proceed from a completely clean base; regeneration of the solvent - ethyl acetate does not present any difficulties (drying with calcium chloride) and the mono acetyl morphine saponification products are not obtained by thickening the mother liquors.
Пример. 1 кг пергкристаллизованного основани раствор ют вExample. 1 kg of percrystallized base is dissolved in
3800 е уксусно-этилового эфира, и раствор охлаждают водой при сильном помешивании. Когда температура раствора понижаетс до 30°, постепенно прибавл ют точно отвешенное, необходимое: по расчету количество абсолютного спирта, насыщенного 36-37% хлористым водородом. Через короткое врем начинает выпадать хлоргидрат, в который переходит и та часть основани , котора выпала из раствора при охлаждении.3800 e of ethyl acetate, and the solution is cooled with water with vigorous stirring. When the temperature of the solution drops to 30 °, gradually weighed, necessary, are gradually added: by calculation, the amount of absolute alcohol saturated with 36-37% hydrogen chloride. After a short time, the hydrochloride begins to precipitate, into which that part of the base that precipitates out of solution upon cooling.
Сразу выпадает хлоргидрата 93% от теории, а остальной получаетс поHydrochloride immediately falls 93% of the theory, and the rest is obtained by
сгущении маточного раствора. Выход количественный.condensation of the mother liquor. The output is quantitative.
II Р Е дм ВТ II л т ; Н т л.II Р Е dm WT II lt; Nt l.
Способ приготовлени хлористсводородного диацетил-морфина (героина), отличающийс тем, что основание диацетил-морфина раствор ют в сухом уксусно-этиловом эфире или смешивают с ним, а необходимый дл образовани соли хлористый водород прибаВ .ЛЯЮТ в виде раствора его в абсолютном спирте.A method of preparing hydrochloric diacetyl-morphine (heroin), characterized in that the diacetyl-morphine base is dissolved in or mixed with dry ethyl acetate and mixed with it, and the hydrochloric acid required for the formation of the salt is dissolved in absolute alcohol.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| SU811-46A SU68594A1 (en) | 1946-04-06 | 1946-04-06 | Method of linking core and molding lands |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| SU811-46A SU68594A1 (en) | 1946-04-06 | 1946-04-06 | Method of linking core and molding lands |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| SU3264A1 true SU3264A1 (en) | 1927-07-30 |
| SU68594A1 SU68594A1 (en) | 1946-11-30 |
Family
ID=48247523
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| SU811-46A SU68594A1 (en) | 1946-04-06 | 1946-04-06 | Method of linking core and molding lands |
Country Status (1)
| Country | Link |
|---|---|
| SU (1) | SU68594A1 (en) |
-
1946
- 1946-04-06 SU SU811-46A patent/SU68594A1/en active
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