Hexane and Acetone are flammable. To pack the column, silica gel was mixed with 14mL of a non-polar solvent, hexane and transferred inside the column.
Field of the Invention The present invention relates to a process for the production of pure fluorenone by oxidation of fluorene fractions with air or oxygen in the presence of quaternary salts.
Description of the Prior Art According to K. However, the process requires a cumbersome processing working up of the alkaline solution by treatment with acids and subsequent extraction with ether for obtaining the fluorenone.
However, production on an industrial scale would be uprofitable because of the required processing of the reaction product connected with large quantities of liquid for the isolation of the fluorenone as well as because of the consumption of fairly large quantities of pyridine.
This process requires special catalysts as well as the traditional measure of melting the fluorene. However, this process requires a higher expenditure of power than is desirable. Finally, it has also been taught in German published application No.
It is therefore a primary object of the present invention to provide a process for the production of pure fluorenone which is equally advantageous from both industrial and economic standpoints.
All of the alkali metal hydroxides can be used. Beyond that, the present process is not comparable with those described above since it takes place in a two-phase system.
This is also the case according to the Soboleva et al.
Hitherto the production was limited to processes in which only aprotic solvents miscible with water such as, for example, pyridine, could be used. The process of the present invention shows that the oxidation is also possible in a suspension of aprotic, solvents immiscible with water, such as for example, methyl naphthalene.
The simultaneous advantage is the saving of solvent which is required in the process of the present invention only in an approximate ratio of 1: In the case of the use of pyridine, on the other hand, higher portions of solvents are necessary.
As a result of the two-phase system used in the present invention, it is possible after completion of the oxidation process to separate the homogeneous organic phase from the inorganic aqueous phase, that is to say, from the alkali metal hydroxide solution.
Since the solvents such as methyl-naphthalene do not dissolve in water, a mixing of the two phases will be avoided. The ratio of organic phase to alkali solution phase is not critical and may generally be from 2: It is therefore possible within the scope of the process of the present invention to distill the fluorenone off directly without further processing of the reaction mixture after the separation of the phases.
With the distillation as the final step, there is the advantage that it is not absolutely necessary to use pure fluorene for the oxidation, but that one may oxidize corresponding fluorene cuts as obtained in the case of tar processing cf.
The methyl naphthalene distilled off may likewise be used for a new oxidation batch. The following non-limiting examples will illustrate the possibilities of the use of various starting products for carrying out the oxidation process of the invention.
After each 10 hours another gram of Triton B was added. After a reaction time of 48 hours, the stirrer mechanism was stopped. The product was allowed to settle and then the homogeneous, organic phase was separated from the inorganic phase. The distillation was conducted with the aid of a tray column under vacuum at a pressure of or 50 mm of mercury.
Claims 8 What is claimed is: The process according to claim 1 wherein after the reaction, the organic phase is separated from the aqueous phase and the pure fluorenone is distilled from said separated organic phase.Fluorenol is an alcohol derivative of fluorene.
In the most significant isomer, fluorenol or 9-hydroxyfluorene, the hydroxy group is located on the bridging carbon between the two benzene rings. Hydroxyfluorene can be converted to fluorenone by oxidation.
Tlc (Fluorene, 9-Fluorenol, 9-Fluorenone) Essay and solvent system on the other. If multiple spots were present for a compound, give Rf value for each component and state if . = Fluorenone, = Fluorene. Flask three was only supposed to have Fluorenone but this shows contamination of the other compound.
For a mixture of fluorene, fluorenone and -fluorenol is examined by TLC and gives the following Rf values: , , | Identify . Separation of Fluorene and 9-Fluorenone. Purpose: Separate a mixture of fluorene and 9 Perform a TLC analysis of the mixture you are about to separate with a solvent mixture of 10% Using a glass Pasteur pipette and bulb add 1 mL of the fluorene/fluoreneone mixuture (prepared from 6 g of each in mL of CH.
2. Cl. 2) solution to the. 9-Fluorenone is used in the preparation of antimalarial drugs. It is a fluorene derivative.
|Specifications||This is because during the reaction, a hydrogen from the borohydride first attaches onto the carbon in the carbonyl group of fluorenone which would leave the oxygen with a negative. In the presence of MeOH, the oxygen would be able to steal the hydrogen from the alcohol group on MeOH which would speed up the reaction as opposed to taking another hydrogen from another borohydride.|
|9-Fluorenone |||In particular, the term 'PAH' refers to the compounds consisting of only carbon and hydrogen atoms while the wider term 'polycyclic aromatic compounds' includes the alkyl-substituted derivatives and functional derivatives such as nitro- and hydroxy-PAH as well as the heterocyclic analogues, which contain one or more hetero atoms in the aromatic structure. PAHs exist in various combinations that manifest various functions such as light sensitivity, heat resistance, conductivity, emittability, corrosion resistance and physiological action.|
|Report Abuse||Fluorene Save Fluoreneor 9H-fluorene, is a polycyclic aromatic hydrocarbon.|
Further, it is used in functional polymer and in dyes. Bemerkungen. 9-Fluorenol, 98+% L Fluorene, 98+% Kürzlich angesehen. Chemikalien. Life science. Metalle und Stoffe. Katalysatoren. The only time 9-fluorenol mobile phase travelled up the silica gel plate is when it was combined with 25% EtOAc in hexane because 75% of the solvent was polar, and the remaining 25% allowed its mobile phase to move up the silica gel plate.
9–fluorenone is the second .