butane

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:145.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Magnesium powder 6.65 gm, (0.273 moles) along with 225.0 ml Isopar "H" hydrocarbon solvent and 0.20 gm of iodine crystals were placed in a 3-necked reaction flask under an argon atmosphere. This mixture was heated under the argon atmosphere to 145° C. for about 60 minutes for metal activation. n-Butyl chloride (40 ml, 0.385 moles) was then gradually added to the reaction slurry in 30 minutes. The heating was cut off due to exothermic reaction and reflux. The reaction of the slurry was continued for about two hours at reflux temperature. The reflux temperature during this period dropped to about 110° C. The reflux solvent contained alkenes (i.e., butene/octene, etc.). After two hours of reaction, heating was cut off and then, the first 15 ml of 2-methyl-1-pentanol of a total of 60 ml was added drop by drop to the reaction slurry. On addition of this alcohol, butane was released with exothermic reaction and the slurry turned into a thick gum-like gel. When the temperature dropped to about 50° C., the remaining 45 ml of 2-methyl-1-pentanol, along with 50 ml of Isopar H solvent, was added quickly under good agitation to reduce the viscosity of the slurry. The 2-methyl-1-pentanol reacted with BuMgCl as was evidenced by the release of butane. The reaction fluid containing some grayish particles was heated slowly with reflux. The reflux butane with some alkene, such as butene/octene, was distilled off through the reflux condenser to increase the reaction temperature close to 145° C. It is important to keep the temperature two to three degrees lower than 2-methyl-1-pentanol's reflux temperature (148° C.-150° C.). The reaction was continued at 145° C. for about 30 minutes. The reaction slurry was filtered while hot (90° C.-120° C.). The filtration was fast and completed in about ten minutes. Final volume of the filtrate was about 340 ml. Fine gray suspended particles of solid were collected on the filter. The clear filtrate was analyzed and found to have a 0.79 molar magnesium concentration with about 98% magnesium recovery. The detailed analysis of the liquid product was found to be 0.79 moles magnesium, 0.50 moles 2MPO (as total base), 1.08 moles chloride per liter, along with solvent Isopar H and excess 2-methyl-1-pentanol. The product formula can be presented as The heating was cut off due to exothermic reaction reflux The reaction of the slurry at reflux temperature The reflux temperature during this period dropped to about 110° C After two hours of reaction heating was released with exothermic reaction When the temperature dropped to about 50° C. The reaction fluid containing some grayish particles was heated slowly with reflux The reflux butane with some alkene, such as butene/octene, was distilled off through the reflux condenser to increase the reaction temperature close to 145° C the temperature two to three degrees reflux temperature (148° C.-150° C.) The reaction was continued at 145° C. for about 30 minutes The reaction slurry was filtered while hot (90° C.-120° C.) The filtration completed in about ten minutes were collected on the filter a 0.79 molar magnesium concentration with about 98% magnesium recovery

反応条件: temp:121.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A reactor equipped witha reflux condenser was charged under an argon atmospher with 6.55 gm of magnesium metal powder (0.269 moles), 250ml. of Isopar "E" isoparaffinic hydrocarbon solvent and a few crystals (0.2 gm) of iodine. This mixture was heated to reflux temperature (121° C.) for about 60 minutes to activate the metal. Then, 28.0 ml (0.27 moles) of n-butyl chloride was added in 30 minutes to this metal slurry at reflux temperature; the resulting reaction mixture was allowed to reflux for 90 minutes. Anhydrous crystalline phenol (C6H5OH) 28 gm (0.298 moles) was then added slowly in melted form along with Isopar E solvent (50° C.) under good agitation. The phenol addition was completed in 20 minutes. During addition of phenol, heating was cut off and maintained at the reflux of released butane from the reaction. The reaction slurry turned from a grayish to a whitish color. The reaction slurry was then heated up to 90° C. with distillation of the refluxing butane. The slurry color turned from gray to white with no visible metal particles. Reaction was continued at 90° C. for another two hours with the addition of another 12 gms (0.128 moles) of phenol. The second addition of phenol was to see if any magnesium solubilized. The hot reaction slurry was then filtered to collect solid product. The solid product was washed with pentane to remove leftover solvents. The filtrate was tested for magnesium and found to be nil. The solid was dried under argon pressure until it was found to be a free flowing powder. Analysis of the solid white product showed 14.82% total magnesium, 56.78% C6H5O, 21.27% Cl, and remaining is free solvent: The filtrate was found to have all the excess phenol in it. This solid white product had an RO/Mg/X (i.e., C6H5O/Mg/Cl) molar ratio almost equal to 1:1:1. A reactor equipped witha reflux condenser This mixture was heated at reflux temperature the resulting reaction mixture to reflux for 90 minutes heating maintained at the Reaction The hot reaction slurry was then filtered to collect solid product The solid product was washed with pentane to remove The solid was dried under argon pressure until it

反応条件: temp:65.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Following the procedure of Example 1, 24.31 gm of magnesium metal powder (1.0 mole) was placed in a 3-necked 3 liter reactor flask, along with 1600 ml of isoparaffinic solvent (Isopar E) having a boiling range of 116°-139° C. and 0.25 gm of iodine crystals. This mixture was heated under an argon atmosphere to reflux temperature for about 60 minutes for metal activation. 105 ml of n-butyl chloride (1.OM) was then gradually added to the reaction slurry in 40 minutes, then reaction was continued for two hours at reflux temperature. Addition of 180 ml (1.4 moles) of 2-methyl-1-pentanol to the reaction slurry was started. The reaction slurry became thick and viscous at reflux temperatures when 60 ml of the 180 ml of the 2-methyl-1-pentanol was added. At this point the reaction slurry was cooled down to 65° C. At 65° C. the remaining 120 ml of 2-methyl-1 -pentanol was added along with 400 ml of solvent (Isopar E) with good agitation to reduce the viscosity of the slurry. The 2-methyl-1-pentanol reacted with BuMgCl as was evidenced by the release of butane. Butane was distilled off through reflux condensor to maintain the reaction temperature close to the reflux temperature of solvent Isopar E. The reaction was continued for two hours. The slurry was filtered while hot, 90°-100° C. The filtration rate was fast and complete in about 10-15 minutes. Final volume of filtrate was about 2100 ml. Fine gray suspended particles as solid were collected on the filter. The clear filtrate was analyzed and found to have 0.435 molar magnesium concentration with 91.40+% magnesium recovery. This filtrate was found to be stable at 0° to 40° C. on storage. was placed in a 3-necked 3 liter reactor flask, along with 1600 ml of isoparaffinic solvent (Isopar E) This mixture was heated under an argon atmosphere to reflux temperature for about 60 minutes for metal activation reaction at reflux temperature was added Butane was distilled off through reflux condensor to maintain the reaction temperature close to the reflux temperature of solvent Isopar E The reaction was continued for two hours The slurry was filtered while hot, 90°-100° C complete in about 10-15 minutes were collected on the filter 0.435 molar magnesium concentration with 91.40+% magnesium recovery to be stable at 0° to 40° C. on storage

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Examples of reactions which can be carried out particularly expediently in the reactors according to the invention are, without this listing being exhaustive: dehydrogenations, for example, of cyclohexylidene-aniline to give diphenylamine and of cyclohexenyl-cyclohexanone to give o-phenylphenol; hydrogenations, for example, of nitrobenzene to give aniline and of phenol to give cyclohexanone; oxidative alcohol dehydrogenations, for example, of 3-methyl-3-buten-1-ol to give 3-methyl-2-buten-1-al; selective oxidations of hydrocarbons, for example, of n-butane to give maleic anhydride, of oxylene to give phthalic anhydride and of propene to give acrolein or acrylic acid and alkylations and halogenations.

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 1759 g (7.65 moles) of 24.2% n-butyllithium in cyclohexane is added over a 90- minute period to 3.70 diisopropylamide and 3.70 moles diisobutyl amine containing 0.3 moles tert butyl alcohol in a 5-liter three-necked flask under nitrogen. The mixture was stirred at a temperature of 20°-30° C. Butane gas evolved during the reaction through an oil by bubbler. The reaction was complete upon final addition of the butyllithium solution. The solution was polish filtered. The final product was 2.7M lithium molar mixed lithium diisopropylamide and diisobutylamide with 3% lithium tert butoxide. filtered mixed lithium diisopropylamide and diisobutylamide with 3% lithium tert butoxide

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 1759 g (7.65 moles) of 24.2% n-butyllithium in cyclohexane is added over a 90- minute period to 3.70 diisopropylamide and 3.70 moles diisobutyl amine containing 0.3 moles tert butyl alcohol in a 5-liter three-necked flask under nitrogen. The mixture was stirred at a temperature of 20°-30° C. Butane gas evolved during the reaction through an oil by bubbler. The reaction was complete upon final addition of the butyllithium solution. The solution was polish filtered. The final product was 2.7M lithium molar mixed lithium diisopropylamide and diisobutylamide with 3% lithium tert butoxide. filtered mixed lithium diisopropylamide and diisobutylamide with 3% lithium tert butoxide

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A fresh sample of niobium promoted VPO catalyst (prepared similarly to the other VPO catalyst used herein but with niobium added during the catalyst preparation) was tested in a 1.5″ diameter steel fluidized bed reactor to determine maleic anhydride yield. The sample was tested at the conditions. Butane conversion and maleic anhydride yield was as listed in Table 1. Note that the yield is higher than for the catalysts in Comparative Examples 2-5. yield

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A fresh sample of niobium promoted VPO catalyst (prepared similarly to the other VPO catalyst used herein but with niobium added during the catalyst preparation) was tested in a 1.5″ diameter steel fluidized bed reactor to determine maleic anhydride yield. The sample was tested at the conditions. Butane conversion and maleic anhydride yield was as listed in Table 1. Note that the yield is higher than for the catalysts in Comparative Examples 2-5. yield