Next we distilled the ethanol before redissolving our product in dichloromethane and washing it with water separatory funnel. Then we distilled the dichloromethane away and ended up with fluorenol, and took IR spectrum. A couple questions, too:
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.characteristics of 9H-fluorene and 9-fluorenone.
2. Look up the density and boiling point of dichloromethane. 3. From the laboratory textbooks in room of the Science Library, read a treatment of thin layer chromatography. In your notebook, write an outline describing how to conduct an analysis by thin layer chromatography.
close up! "If you want a close-up view you should move yourself if it is possible. The trouble is that so many photographers seem afraid to move in." (Lord Snowdon) How can moving close to a subject change and improve a photograph?
Tlc (Fluorene, 9-Fluorenol, 9-Fluorenone) other. If multiple spots were present for a compound, give Rf value for each component and state if .
9-fluorenone is different because it is a ketone with all of its carbons tied up in double bonds. There are no readily available acidic hydrogens, therefore this makes the pka of the molecule much greater than most other ketones.
Other names: 9-Hydroxyfluorene; 9-Fluorenol; Diphenylene carbinol; Fluorenol; Fluorenol; 9H-Fluoreneol Permanent link for this species. Use this link . Fluorenol Buy Fluorenol Fluorenol User Reviews Contact Fluorenol Buy Fluorenol Fluorenol User Reviews Contact Fluorenol Safety.
Direct Fuorenol Source. Fluorenol Safety Date Sheet. Powered by Create your own unique website with customizable templates. Get Started.