US1123522A - Process of preparing nicotin. - Google Patents

Process of preparing nicotin. Download PDF

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Publication number
US1123522A
US1123522A US77069413A US1913770694A US1123522A US 1123522 A US1123522 A US 1123522A US 77069413 A US77069413 A US 77069413A US 1913770694 A US1913770694 A US 1913770694A US 1123522 A US1123522 A US 1123522A
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Prior art keywords
nicotin
tobacco
preparing
solvent
salts
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US77069413A
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Walter Halle
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07DHETEROCYCLIC COMPOUNDS
    • C07D401/00Heterocyclic compounds containing two or more hetero rings, having nitrogen atoms as the only ring hetero atoms, at least one ring being a six-membered ring with only one nitrogen atom
    • C07D401/02Heterocyclic compounds containing two or more hetero rings, having nitrogen atoms as the only ring hetero atoms, at least one ring being a six-membered ring with only one nitrogen atom containing two hetero rings
    • C07D401/04Heterocyclic compounds containing two or more hetero rings, having nitrogen atoms as the only ring hetero atoms, at least one ring being a six-membered ring with only one nitrogen atom containing two hetero rings directly linked by a ring-member-to-ring-member bond

Definitions

  • This invention relates to a process. of preparing nicotin and has for its object to extract nicotin from the tobacco directly, that is to say without any preliminary preparation or processes such as have heretofore been necessary.
  • N icotin as is well known, is almost exclusively combined with organic acids in tobacco, that is, ,in the form of salts and not asfree base. 11 order to obtain the base by extraction with an easily volatile solvent, it
  • nicotin salts are thereby decomposed into their components and the nicotin is distilled in an almost pure state into the receiver.
  • nicotin In tliismanner nic otin can be isolated by means-of simple distillation from the extract in which it is contained besides an abundant. quantity of other substances such as resin-like bodies, wax, and the like; and this can be done directly without the round-about way of preparing first the. oxalate or similar complicated methods at purification.
  • nicotin which can be'obtaine'd quite pure by re-distillation in a current of hydrogen in a high Vacuum.
  • the variable content in nicotin is a result of the variable composition of the difi erent kinds of tobacco.
  • the present process is considerably simpl r as compared with the hitherto used processes. Only by this process the problem of manufacturing nicotin on an industrial scale in a satisfactory manner is solved. and the possibility of utilizing tobacco waste on a commercial scale for the production of nicotin is-made practicable by the present invention.
  • a process of consists in extracting tobacco by means of an organic solvent, without decomposition of the nicotin salts by alkalis, evaporating the'solvent, and subjecting the obtained extract to distillation in vacuum.
  • a process of obtaining nicotin comprising treating'tobacco with an organic solvent to directly extract the nicotin salts contained therein, evaporating the'sdlvent, treating the residue to decompose the nicotin salts into their the nicotin.
  • a process of obtaining nicotin comprising treating tobacco with an organic sol vent to extract therefrom undecomposed form, evaporating the solvent, and treating the residue to separate the nicotin therefrom.
  • a process of preparing nicotin from tobacco waste having itsfnicotin salts unpreferably solid tobacco is extracted after suit- .(p'ei'chloromethane).
  • a process of preparing nicotin comprising treating tobacco with-a" benzene soling the-residue -waste while retaining its nicotin salts un-i vent, evaporating the .-solvent;, and subjecttodisti llation in vacuum.
  • a process of extracting tobacco waste which comprises comminuting said tobacco 'in which said tobacco -while still in a condition in which it redecorriposedby alkalis, treating said comminuted tobacco waste in the said state by means ofan organic solvent, and distilling.
  • a process of extracting tobacco waste Waste is comminuted waste in said condition by means of an organic solvent, evaporating said solvent, and subjecting the extract thus obtained to distillation.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Manufacture Of Tobacco Products (AREA)

Description

masses.
No Drawing.
7 To all whom it may cohcrn:
Be it known that I, VVALTER HALLE, a subject of the Emperor ofwAustria-Hungary, residing at Budapest, Austria- Hungary, have invented new and useful llm'prove ments in Processes of Preparing Nicotin, of which the following isa specification.
This invention relates to a process. of preparing nicotin and has for its object to extract nicotin from the tobacco directly, that is to say without any preliminary preparation or processes such as have heretofore been necessary.
N icotin, as is well known, is almost exclusively combined with organic acids in tobacco, that is, ,in the form of salts and not asfree base. 11 order to obtain the base by extraction with an easily volatile solvent, it
is therefore necessary to free it from the salts by means of alkalis. Fromthe'solutions obtained in this manner nicotin according to processes hitherto in use was obtained in a verytroublesome way. In most cases the base had'to be precipitated as oxalate by shaking the solution with oxalic acid. This salt had to be purified by means of several operations, and after this the nicotin was liberated and eventually purified by distillation ina current'of hydrogen.
Almost all other known processes and also those which start from aqueous tobacco extracts proceed on the same lines, the nicotin being in all these processes, obtained in the form of the-oxal'ate-oranother salt. The step from the crude nicotin salt to pure nicotin is, however, a very considerable one, with which is associated a loss in yieldexceeding per cent. In contra-distinctionto these known processes according to the present invention the nicotin is extracted from tobacco by means of suitable organic solvents, in the form of its salts without previous liberation of" thebase. After evaporating the solvent the residue is subjected to distillation in vacuum. The nicotin salts are thereby decomposed into their components and the nicotin is distilled in an almost pure state into the receiver. In tliismanner nic otin can be isolated by means-of simple distillation from the extract in which it is contained besides an abundant. quantity of other substances such as resin-like bodies, wax, and the like; and this can be done directly without the round-about way of preparing first the. oxalate or similar complicated methods at purification. For carrying out the process,
Specification of Letters Patent.
.to about 140.
. the nico PROCESS OF PREPARING NICOTIN.
residue remaining after evaporation of the solvent is fractionated in a suitable distillation vessel under reduced pressure (for example 12 to 15 mm); running the temperature of the vapor rises The main fraction which passes over contains 80 to 98 per cent. of nicotin, which can be'obtaine'd quite pure by re-distillation in a current of hydrogen in a high Vacuum. The variable content in nicotin is a result of the variable composition of the difi erent kinds of tobacco. The present process is considerably simpl r as compared with the hitherto used processes. Only by this process the problem of manufacturing nicotin on an industrial scale in a satisfactory manner is solved. and the possibility of utilizing tobacco waste on a commercial scale for the production of nicotin is-made practicable by the present invention.
I claim: 1. A process of consists in extracting tobacco by means of an organic solvent, without decomposition of the nicotin salts by alkalis, evaporating the'solvent, and subjecting the obtained extract to distillation in vacuum.
process of obtaining nicotin comprising treating tobacco to directly extract tin salts contained therein, and subjecting the obtained in vacuum. 7, v
3. A process of obtaining nicotin comprising treating'tobacco with an organic solvent to directly extract the nicotin salts contained therein, evaporating the'sdlvent, treating the residue to decompose the nicotin salts into their the nicotin. V v
4.. A process of obtaining nicotin comprising treating tobacco with an organic sol vent to extract therefrom undecomposed form, evaporating the solvent, and treating the residue to separate the nicotin therefrom.
A process of preparing nicotin from tobacco waste having itsfnicotin salts unpreferably solid tobacco is extracted after suit- .(p'ei'chloromethane).
After a small first preparing nicotin which extract, to distillation components, and collecting I nicotin" salts in lPatented Jane, T9115. Application filed May 29, 1913. Serial No. 770,694.
decomposed alkalis,
comprising comminuting said tobacco waste, extracting said comminuted tobacco waste by'means of an organic solvent, evaporating the solvent, and distilling in vacuum the extract thus ob: tained.
6. A process of preparing nicotin. which i consists in extracting dry tobacco by means "vacuum;
1 r pr sing treatingtobacco with 'a solvent conof a solventcomprising a mixture of benzin' and benzene, without previous decomposition. of the nicotin fsalts by alkalis, evaporating the solvent, and sub]ecting the extract thus obtained to distillation in -7.. A process of preparing nicotin" com taining benzene, evaporating the solvent,
" treating the residue to decompose the nicotin' salts into their components, and collectingf the nicotin. I Y
8. A process of preparing nicotin comprising treating tobacco with-a" benzene soling the-residue -waste while retaining its nicotin salts un-i vent, evaporating the .-solvent;, and subjecttodisti llation in vacuum.
9. A process of extracting tobacco waste which comprises comminuting said tobacco 'in which said tobacco -while still in a condition in which it redecorriposedby alkalis, treating said comminuted tobacco waste in the said state by means ofan organic solvent, and distilling.
the extract thus obtained in vacuum.
'10. A process of extracting tobacco waste Waste is comminuted waste in said condition by means of an organic solvent, evaporating said solvent, and subjecting the extract thus obtained to distillation.
.- 7 WALTER HALLE. Witnesses:
-JosnPH G. STADLER, AUGUST FUGGER.
US77069413A 1913-05-29 1913-05-29 Process of preparing nicotin. Expired - Lifetime US1123522A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE1069478B (en) *
US3096773A (en) * 1957-04-12 1963-07-09 Sasmoco Sa Process for treating tobacco and tobacco obtained by said process
US3394709A (en) * 1964-04-13 1968-07-30 Inca Inks Treatment of tobacco

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE1069478B (en) *
US3096773A (en) * 1957-04-12 1963-07-09 Sasmoco Sa Process for treating tobacco and tobacco obtained by said process
US3394709A (en) * 1964-04-13 1968-07-30 Inca Inks Treatment of tobacco

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