The Benzophenone
The Benzophenone
A, na + diphenyl ketone in addition to the principle of waterBenzophenone
A, na + diphenyl ketone in addition to the principle of water
Diphenyl ketone as indicator in the synthetic experiments are very versatile, can be used as a treatment of toluene, benzene, THF, acetonitrile and other indicator;After join if appeared a beautiful blue, can use distillation, its reason: the free radical anion generated by a ketone was called carbonyl free radicals, diphenyl ketone indicator is diphenyl ketone of oxygen seized the sodium, the electrons in generating the dark carbonyl free radicals;The free radicals on the stereo, electrical aspects is stable, mainly used to indicate the anaerobic condition.After adding diphenyl ketone, solution of the blue, show the oxygen in solution is less, the indirect water rarely.But is blue, and join the diphenyl ketone and deal with the amount of solvent, THF (300 ml) of water, about 6 hours to return, related to deal with the amount of solvent, of course, the more you have, the longer toluene, benzene and other water reflux time less and less time will be shortened.
2, na + diphenyl ketone in addition to water steps
1: the presence of peroxide method one: to take a small amount of reagent (diethyl ether and tetrahydrofuran) and 2% of potassium iodide solution volume, add a few drops of dilute hydrochloric acid with vibration wave, purple or blue, if you can make the starch solution is proved that the presence of peroxide.Method 2: using starch potassium iodide dipstick test peroxide exists.Remove peroxide reagent can be added in the separatory funnel and size 1/5 new reagent in ferrous sulfate solution, points to aqueous solution after shaking.
2: to water to add common desiccant, such as: potassium carbonate, sodium sulfate, sodium hydroxide, such as pretreatment or with 4 a molecular sieve (high temperature to dry for several hours), to water for a few days;
3: connection handles stay solvent added to the flask, connection device, stirring, bubbled into nitrogen;4: add sodium metal operation method: take sodium metal, use a knife to cut to oxidized surface, then slice, use scissors to cut into filaments, into the small beaker, added to the flask with forceps, pay attention to a few times;Operation method 2: use clean reagent bottles or other things into slices, then use scissors;If you have experimental conditions can make sodium sand, sodium beads;5: questions about adding sodium 500 ml solvent plus two pieces of sodium of nail size is enough, by feeling, more less it doesn't matter;If there is no hydrogen is produced.After a while nitrogen can add nitrogen to the ball.6: plus diphenyl ketone and metallic sodium reflux after a period of time (4 hours) and diphenyl ketone, diphenyl ketone 500 ml of solvent add a spoonful of left and right sides is enough, it is a indicator does not need too much.7: steamed out after solvent liquid blue, can be recycled.If there is the same blue, may be a reflux time too short, bottle contains oxygen.Part of distillation in the end, to be kept to prevent high temperature peroxides explosion.8: the processing of residual sodium with petri dishes or beakers into ethanol, the rest of the sodium added to ethanol with a pair of tweezers [http://www.guidechem.com/cas-119/119-61-9.html], to a few times.Sodium until disappear.
A, na + diphenyl ketone in addition to the principle of waterBenzophenone
A, na + diphenyl ketone in addition to the principle of water
Diphenyl ketone as indicator in the synthetic experiments are very versatile, can be used as a treatment of toluene, benzene, THF, acetonitrile and other indicator;After join if appeared a beautiful blue, can use distillation, its reason: the free radical anion generated by a ketone was called carbonyl free radicals, diphenyl ketone indicator is diphenyl ketone of oxygen seized the sodium, the electrons in generating the dark carbonyl free radicals;The free radicals on the stereo, electrical aspects is stable, mainly used to indicate the anaerobic condition.After adding diphenyl ketone, solution of the blue, show the oxygen in solution is less, the indirect water rarely.But is blue, and join the diphenyl ketone and deal with the amount of solvent, THF (300 ml) of water, about 6 hours to return, related to deal with the amount of solvent, of course, the more you have, the longer toluene, benzene and other water reflux time less and less time will be shortened.
2, na + diphenyl ketone in addition to water steps
1: the presence of peroxide method one: to take a small amount of reagent (diethyl ether and tetrahydrofuran) and 2% of potassium iodide solution volume, add a few drops of dilute hydrochloric acid with vibration wave, purple or blue, if you can make the starch solution is proved that the presence of peroxide.Method 2: using starch potassium iodide dipstick test peroxide exists.Remove peroxide reagent can be added in the separatory funnel and size 1/5 new reagent in ferrous sulfate solution, points to aqueous solution after shaking.
2: to water to add common desiccant, such as: potassium carbonate, sodium sulfate, sodium hydroxide, such as pretreatment or with 4 a molecular sieve (high temperature to dry for several hours), to water for a few days;
3: connection handles stay solvent added to the flask, connection device, stirring, bubbled into nitrogen;4: add sodium metal operation method: take sodium metal, use a knife to cut to oxidized surface, then slice, use scissors to cut into filaments, into the small beaker, added to the flask with forceps, pay attention to a few times;Operation method 2: use clean reagent bottles or other things into slices, then use scissors;If you have experimental conditions can make sodium sand, sodium beads;5: questions about adding sodium 500 ml solvent plus two pieces of sodium of nail size is enough, by feeling, more less it doesn't matter;If there is no hydrogen is produced.After a while nitrogen can add nitrogen to the ball.6: plus diphenyl ketone and metallic sodium reflux after a period of time (4 hours) and diphenyl ketone, diphenyl ketone 500 ml of solvent add a spoonful of left and right sides is enough, it is a indicator does not need too much.7: steamed out after solvent liquid blue, can be recycled.If there is the same blue, may be a reflux time too short, bottle contains oxygen.Part of distillation in the end, to be kept to prevent high temperature peroxides explosion.8: the processing of residual sodium with petri dishes or beakers into ethanol, the rest of the sodium added to ethanol with a pair of tweezers [http://www.guidechem.com/cas-119/119-61-9.html], to a few times.Sodium until disappear.
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