Neodecanoic acid

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:; See reaction.notes.procedure_details.

実験手順: Ammonia liquor (SG 0.88, 36 ml, 0.6 mole) was added dropwise to neodecanoic acid (95%, 103.2 g, 0.6 mole; Exxon purified by vacuum distillation) in ice-cooled distilled water (200 ml). The resulting ammonium neodecanoate soap was stirred at ambient temperature for 90 minutes, and then silver nitrate (101.94 g. 0.6 mole) in distilled water (120 ml) was added dropwise. The resultant white semi-solid was tritrated 4 times each with cold and warm (50° C.) distilled water, slurried in methanol (400 ml), filtered off and dried overnight at 40° C. under vacuum. Contains 30 wt% silver; yield 64% w.r.t. silver. cooled distilled water (200 ml) warm (50° C.) distilled water filtered off dried overnight at 40° C. under vacuum r.t. silver

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

実験手順: A silver neo-decanoate/cumene solution is prepared from 539.00 gm of neo-decanoic acid (obtained from Exxon Chemical Co.), 350.00 gm of cumene (obtained from Aldrich Chemical Co.), and an excessive amount of silver oxide (392.21 gm) in a similar manner to that described in Example 1 of U.S. Pat. No. 4,663,303. A 496.42 gm sample of this solution is diluted with 19.35 gm of cumene to yield a solution having a weight ratio of silver salt/cumene of 2.2/1.0. to yield a solution

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

実験手順: A silver neo-decanoate/cumene solution is prepared from 539.00 gm of neo-decanoic acid (obtained from Exxon Chemical Co.), 350.00 gm of cumene (obtained from Aldrich Chemical Co.), and an excessive amount of silver oxide (392.21 gm) in a similar manner to that described in Example 1 of U.S. Pat. No. 4,663,303. A 496.42 gm sample of this solution is diluted with 19.35 gm of cumene to yield a solution having a weight ratio of silver salt/cumene of 2.2/1.0. to yield a solution

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

実験手順: Silver neodecanoate was prepared according to the procedure as disclosed in Armstrong, U.S. Pat. No. 4,555,501 herein incorporated by reference, from silver (I) oxide and neodecanoic acid. A slurry of 5 ml neodecanoic acid and 5 ml absolute ethanol was heated to 80° C. in an oil bath. Approximately 1.7 grams Ag2O was added slowly and the resulting solution was heated for approximately 5 minutes. One drop of 30 percent by weight H2O2 was added to the resulting solution to oxidize any prereduced silver metal. After the addition of H2O2 the solution was clear yellow. Absolute ethanol was added to the solution to precipitate white silver neodecanoate. The precipitate was filtered and reslurried twice in absolute ethanol. An amount of the dye, 3,3'-di(3-acetoxypropyl-11-diphenylamino-10,12-ethylene-5,5',6,6'-dibenzothiatricarbocyanine perchlorate) was added to a methylene chloride solution to provide a 0.01 molar solution. To this solution was added 1 weight percent silver neodecanoate and 1 weight percent polystyrene, based upon the weight of the solution. This solution was spin-coated onto a glass substrate to provide an active layer approximately 1 μm thick. the resulting solution was heated for approximately 5 minutes to precipitate white silver neodecanoate The precipitate was filtered An amount of the dye, 3,3'-di(3-acetoxypropyl-11-diphenylamino-10,12-ethylene-5,5',6,6'-dibenzothiatricarbocyanine perchlorate) was added to a methylene chloride solution

反応条件: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 1 g of 7,7-dimethyloctanoic acid is dissolved in 20 ml of DCM cooled to 0° C., 0.57 ml of oxalyl chloride is added and the mixture is then left stirring for 1 hour at 0° C. and for 2 hours at RT. 0.93 ml of 2,5-dimethoxytoluene and one drop of DMF are added, the mixture is cooled to 0° C., 940 mg of AlCl3 are then added and the mixture is left stirring for 1 hour at 0° C. and overnight at RT. It is poured into 10% HCl solution and extracted with ether, and the combined organic phases are then washed with 2N sodium hydroxide, dried and concentrated. The residue is chromatographed on silica, eluting with DCM/pentane (85/15; v/v) to give 1.05 g of the expected compound. the mixture is then left the mixture is cooled to 0° C. the mixture is left stirring for 1 hour at 0° C. and overnight at RT extracted with ether the combined organic phases are then washed with 2N sodium hydroxide dried concentrated The residue is chromatographed on silica eluting with DCM/pentane (85/15; v/v)

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

実験手順: Ammonia liquor (SG 0.88, 36 ml, 0.6 mole) was added dropwise to neodecanoic acid (95%, 103.2 g, 0.6 mole; Exxon purified by vacuum distillation) in ice-cooled distilled water (200 ml). The resulting ammonium neodecanoate soap was stirred at ambient temperature for 90 minutes, and then silver nitrate (101.94 g. 0.6 mole) in distilled water (120 ml) was added dropwise. The resultant white semi-solid was tritrated 4 times each with cold and warm (50° C.) distilled water, slurried in methanol (400 ml), filtered off and dried overnight at 40° C. under vacuum. Contains 30 wt% silver; yield 64% w.r.t. silver. cooled distilled water (200 ml) warm (50° C.) distilled water filtered off dried overnight at 40° C. under vacuum r.t. silver

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

実験手順: A silver neo-decanoate/cumene solution is prepared from 539.00 gm of neo-decanoic acid (obtained from Exxon Chemical Co.), 350.00 gm of cumene (obtained from Aldrich Chemical Co.), and an excessive amount of silver oxide (392.21 gm) in a similar manner to that described in Example 1 of U.S. Pat. No. 4,663,303. A 496.42 gm sample of this solution is diluted with 19.35 gm of cumene to yield a solution having a weight ratio of silver salt/cumene of 2.2/1.0. to yield a solution

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

実験手順: A silver neo-decanoate/cumene solution is prepared from 539.00 gm of neo-decanoic acid (obtained from Exxon Chemical Co.), 350.00 gm of cumene (obtained from Aldrich Chemical Co.), and an excessive amount of silver oxide (392.21 gm) in a similar manner to that described in Example 1 of U.S. Pat. No. 4,663,303. A 496.42 gm sample of this solution is diluted with 19.35 gm of cumene to yield a solution having a weight ratio of silver salt/cumene of 2.2/1.0. to yield a solution

反応条件: temp:100.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To a one liter stainless steel autoclave, equipped with a mechanical stirrer, heater, cooling coils, automatic temperature controller, and a tared ethylene oxide cylinder, in a series of runs is added 500 grams neodecanoic acid and 2.0 g of the selected catalyst. The reactor is heated to approximately 100° C. and a gaseous N2 purge of the reactor is introduced to remove both oxygen and water. With continued N2 purging its temperature of the neo acid/catalyst solution is gradually raised to 150° C. Upon reaching temperature, the N2 purge is stopped and the reactor vents are sealed. Ethylene oxide is then slowly added to the reactor to maintain a reactor pressure of about 30 psig. The flow of ethylene oxide is then stopped. The reaction mixture is stirred for an additional 20 minutes, until the reactor pressure decreases to 15 psig. Total reaction time, from the start of ethylene oxide addition is about 55 minutes. The reactor is then vented, a gaseous nitrogen purge is introduced, and the reaction product is cooled to room temperature. The crude ethylene glycol mononeodecanoate product mixture thereby obtained was analyzed by gas chromatography. The data obtained are set forth in Table II below. heater, cooling coils, automatic temperature controller a gaseous N2 purge of the reactor is introduced to remove both oxygen and water With continued N2 purging its temperature of the neo acid/catalyst solution is gradually raised to 150° C the N2 purge the reactor vents are sealed Ethylene oxide is then slowly added to the reactor to maintain a reactor pressure of about 30 psig Total reaction time, from the start of ethylene oxide addition is about 55 minutes a gaseous nitrogen purge is introduced the reaction product is cooled to room temperature

反応条件: temp:0.00; pressure:0.00; stir: